Tag: M.W:0-100

872-32-2, 2-Methyl-1-pyrroline is a pyrrolines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,872-32-2

General procedure: 4-Chloro-benzenesulfonyl chloride (6.33 g, 30 mmol) was added to a solution of 4-dimethylaminopyridine (DMAP) (3.67 g, 30 mmol) in anhydrous DMF (25 mL) at 0 ¡ãC. The reaction was stirred at 23¡ã C for 30 minutes. A solution of 2-methyl-l-pyrroline (2.08 g, 25 mmol) in anhydrous DMF (25 mL) was added and the reaction was stirred at the same temperature for 1 hour. Methanesulfonic acid (4.87 mL, 75 mmol) was added to the reaction at 0 ¡ãC. The reaction was then stirred at 23¡ã C for 2 hours. 4-Bromo-2-fluoro-phenyl hydrazine hydrochloride (9.06 g, 35.7 mmol) was added and stirred for an additional hour at 23¡ã C. The reaction was then heated to 85 ¡ãC for 12 hours in a sealed tube. The reaction was then cooled to room temperature and concentrated in vacuo. The resulting residue was dissolved in ethyl acetate and washed with saturated aqueous solution of NaHC03 followed by brine. The combined organic layers were dried over anhydrous Na2S04; filtered and concentrated in vacuo to give a crude product, which was purified by column (0241) chromatography on silica gel eluting with 70:30 Hex: EtOAc to give N-(2-(5-bromo-7-fluoro- 2-methyl-lH-indol-3-yl)ethyl)-4-chlorobenzenesulfonamide (SI) as an off-white solid

The synthetic route of 872-32-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; THE REGENTS OF THE UNIVERSITY OF COLORADO, A BODY CORPORATE; WANG, Xiang; BARBOUR, Patrick; (44 pag.)WO2016/176634; (2016); A1;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.872-32-2,2-Methyl-1-pyrroline,as a common compound, the synthetic route is as follows.

General procedure: Acyl chloride (1.2 mmol, 1.2 equiv) was added to a solution of 4-dimethylaminopyridine (DMAP) (1.2 mmol, 1.2 equiv) in acetonitrile (1.0 mL) at 0 ¡ãC. The reaction was stirred at room temperature for 15 min. A solution of the 5-methyl-3,4-dihydro-2H-pyrrole (1.0 mmol) in acetonitrile (1.0 mL) was added and the reaction was stirred at room temperature for 3 h. p-Toluenesulfonic acid monohydrate (3.0 mmol, 3.0 equiv) was added at 0 ¡ãC under inert atmosphere. The reaction was then stirred at room temperature for 2 h. Arylhydrazine (1.5 mmol, 1.5 equiv) was added and stirred for an addition 5 min at room temperature. The reaction was then heated to 82 ¡ãC for 20 h. The reaction cools down to room temperature. The residue was then dissolved in ethyl acetate and washed with brine and a saturated aqueous solution of NaHCO3. The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated in vacuo to give a crude solid, which was purified by column chromatography on silica gel., 872-32-2

872-32-2 2-Methyl-1-pyrroline 70103, apyrrolines compound, is more and more widely used in various fields.

Reference£º
Article; Yeo, Se Jeong; Liu, Yongxiang; Wang, Xiang; Tetrahedron; vol. 68; 3; (2012); p. 813 – 818;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

872-32-2, 2-Methyl-1-pyrroline is a pyrrolines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

872-32-2, Intermediate 1: Methyl 3-chloro-lH-pyrrole-2-carboxylate At 55-60 ¡ãC with vigorous stirring to a mixture of NCS (107 g, 800 mmol) in THF (250 mL) in a 2 L flask was added 5-methyl-3,4-dihydro-2H-pyrrole (8.3 g, 100 mmol) in one-portion. After addition, the reaction spontaneously heated to reflux for about 5 min, then reacted at 60-70 ¡ãC for another 1.5 hours. After cooled to r.t., hexane (300 mL) and water (300 mL) were added to the mixture. The organic layer was separated, collected and concentrated. The residue was used in the next step without further purification. To a mixture of the crude 4,4-dichloro-5-(trichloromethyl)-3,4-dihydro-2H-pyrrole (240 g, 941 mmol) in MeOH (2 L) in an ice-bath was added a solution of NaOMe (324 g, 6 mol) in MeOH (1.5 L) drop-wise over an hour. After addition, the mixture was stirred at r.t. for another one hour. Then 2N HCl aq. was added to adjust its pH to 2 and the resulting was stirred at room temperature for 15 minutes. The mixture was concentrated and diluted with EtOAc (2.5 L) and water (2 L). The organic layer was separated, concentrated and purified by column chromatography eluting with EtOAc/PE and then crystallize upon standing. Methyl 3-chloro-lH-pyrrole-2-carboxylate was obtained as an orange solid (91.3 g, yield: 61percent). MS (m/z): 160.1 (M+H)+ . 1H NMR (400 MHz, DMSO-de) delta 12.05 (s, 1H), 6.98 (m, 1H), 6.21 (t, / = 2.6 Hz, 1H), 3.75 (s, 3H).

The synthetic route of 872-32-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; HUTCHISON MEDIPHARMA LIMITED; SU, Wei-Guo; DAI, Guangxiu; XIAO, Kun; JIA, Hong; VENABLE, Jennifer Diane; BEMBENEK, Scott Damian; WO2014/15675; (2014); A1;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.872-32-2,2-Methyl-1-pyrroline,as a common compound, the synthetic route is as follows.

5-Methyl-3,4-dihydro-2H-pyrrole (60.2 mmol, 1.0 equiv.) was dissolved in CCl4 (100 ml); at 0¡ã C., N-chlorosuccinimide (8.0 equiv.) was added in portions, and the mixture was heated for 72 h at boiling temperature. The reaction mixture was cooled to 0¡ã C., and the resulting solid was filtered out and washed with cooled (0¡ã C.) CCL4 (2.x.50 ml). The filtrate was concentrated to dryness under reduced pressure. Yield: 90percent, 872-32-2

The synthetic route of 872-32-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Gruenenthal GmbH; US2010/222324; (2010); A1;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.872-32-2,2-Methyl-1-pyrroline,as a common compound, the synthetic route is as follows.

872-32-2, 5-methyl-3,4-dihydro-2H-pyrrole (4 g, 0.05 mol) was dissolved in THF (120 mL) and N-chlorosuccinimide (51.4 g, 0.39 mol) was slowly added at 0 ¡ã C and refluxed for 15 minutes. The reaction mixture was stirred at 70 & lt; After stirring for two and a half hours, the THF was removed under reduced pressure, extracted three times with dichloromethane and washed with brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure to obtain 4,4-dichloro-5- (trichloromethyl) -3,4-dihydro-2H-pyrrole.It was used immediately for the next reaction without further purification. 4,4-Dichloro-5- (trichloromethyl) -3,4-dihydro-2H-pyrrole (2 ) (12 g, 0.05 mol) To methanol (100 mL) was added And dissolved in sodium methoxide (NaOMe) (28 wtpercent methanol) (16 g, 0.29 mol) is slowly added dropwise at 0 . The reaction mixture was reacted at room temperature for 2 hours, extracted three times with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The reaction mixture was purified by flash column chromatography (n-hexane: ethyl acetate = 5: 1) Purification yielded 6.5 g (0.04 mol, 77percent yield) of brown solid compound methyl 3-chloro-lH-pyrrole-2-carboxylate.

As the paragraph descriping shows that 872-32-2 is playing an increasingly important role.

Reference£º
Patent; Korea Research Institute of Chemical Technology; Lee, Gay Hyung; Lim, Hee Jong; Cho, Hee Young; Park, Woo Kyu; Jung, Dae Young; (40 pag.)KR2017/74381; (2017); A;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.541-59-3,Maleimide,as a common compound, the synthetic route is as follows.,541-59-3

Example 9:conversion of an amine to a maleimide moiety /V-(Methoxycarbonyl)maleimide (37) Methyl chloroformate (0.87 ml_, 11.3 mmol) was added slowly to a solution of maleimide (1.00 g, 10.3 mmol) and /V-methyl morpholine (1.24 ml_, 1 1.3 mmol) in EtOAc (80 ml_) at 0 C and stirred for 1 hr. The precipitate was separated out through filtration through a celite pad and the filtrate concentrated in vacuo. It was attempted to recrystallise the crude oil with hexane: CH2CI2 but no crystallisation occurred. The crude product was redissolved in EtOAc (100 ml_), adsorbed onto silica and purified using column chromatography (Hex: EtOAc 6:4) to yield a white solid (1 .07 g, 67%). 5H (CDCI3, 300 MHz): 6.83 (2H, s, CH-3/4), 3.94 (3H, s, CH3-2′) 8c (CDCI3, 100 MHz): 165.6 (C-2/5), 148.1 (C-1 ‘), 132.3 (C-3/4), 54.2 (C-2’)

541-59-3 Maleimide 10935, apyrrolines compound, is more and more widely used in various fields.

Reference£º
Patent; THE SOUTH AFRICAN NUCLEAR ENERGY CORPORATION LIMITED; UNIVERSITY OF CAPE TOWN; DRIVER, Cathryn Helena Stanford; ZEEVAART, Jan Rijn; PARKER, Mohamed Iqbal; HUNTER, Roger; (67 pag.)WO2016/46793; (2016); A2;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.541-59-3,Maleimide,as a common compound, the synthetic route is as follows.

541-59-3, Preparation 1: 3-(4-bromophenyl)-1H-pyrrole-2,5-dione (P1) A solution of hydrochloric acid (37percent, 27 ml.) in water (11 ml_) was added to 4-bromo aniline (15 g) at room temperature with vigorous stirring and the formed precipitate was allowed to stir for further 30 minutes. Temperature was reduced to 0 0C and a solution of sodium nitrite (6.60 g) in water (17 ml_) was added dropwise to the stirred suspension. At the end of diazotisation, a clear yellow solution was obtained. Maleimide (16.90 g) in acetone (70 mL) was added dropwise at 0 0C and then the pH of the solution was adjusted to 3-3.5 by adding sodium acetate. Copper (II) chloride (1.76 g) was added to the vigorously stirred mixture. The reaction mixture was allowed to stir at 0 0C for 1 h and overnight at room temperature. Acetone was removed in vacuo, the residue was filtered and dried overnight in vacuo to give the crude title compound (14.12 g) which was used without further purification.MS (mlz): 251 [M-H]”.

The synthetic route of 541-59-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GLAXO GROUP LIMITED; WO2007/22935; (2007); A1;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

541-59-3,541-59-3, Maleimide is a pyrrolines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Methylchloroformate (4.4 niL, 56.7 mmol, 1 eq) was added to a solution of maleimide (5.5 g, 56.7 mmol, 1 eq) and NMM (6.2 mL, 56.7 mmol, 1 eq) in 200 niL of EtOAc at 0 0C. The suspension was stirred at 0 C for 30 minutes, filtered and washed with EtOAc. Filtrate and washings were combined and washed with cold water and dried over anhydrous Na2SO4. After filtration and evaporation under vacuum a pink solid was obtained. Purification by column chromatography on silica gel (Hexane-EtOAc, 1:1, v/v) provided the product (4.8 g, 55%).

As the paragraph descriping shows that 541-59-3 is playing an increasingly important role.

Reference£º
Patent; ENZON PHARMACEUTICALS, INC.; WO2008/34124; (2008); A2;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.541-59-3,Maleimide,as a common compound, the synthetic route is as follows.,541-59-3

Example 1 Preparation of N-Methoxycarbonylmaleimide STR13 To a 1000 ml 3-neck round bottom flask was added 400 ml of ethyl acetate. The flask was placed in an ice bath and the temperature was allowed to drop to about 0 C. To the cooled flask was sequentially added with stirring 7.76 g of maleimide and 8.8 ml of N-methylmorpholine. Then, through an addition funnel was added to the stirring mixture 6.26 ml of methyl chloroformate at a rate so as not to raise the temperature above 3 C. Through the addition funnel was then added 5 ml of ethyl acetate as washing and the washing was added to the reaction mixture. The reaction mixture was stirred for 30 minutes at between 0-3 C. Thereafter, the reaction mixture was filtered through a Buchner funnel. The flask was washed 2* with 10 ml of ethyl acetate and the washings were also filtered. The resulting precipitate was washed 2*with 10 ml of ethyl acetate. The combined filtrate and washings were extracted with 100 ml of ice cold water, dried (10 g Na2 SO4), and evaporated to dryness under reduced pressure.

As the paragraph descriping shows that 541-59-3 is playing an increasingly important role.

Reference£º
Patent; Hybritech Incorporated; US5091542; (1992); A;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem

541-59-3, Maleimide is a pyrrolines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,541-59-3

The title compound was prepared using a modification of the method of Foley, et al., 2010 Biomol. Chem. 8:4601-4606). To a solution of maleimide (5.0 g, 51.5 mmole) in dry ethyl acetate (250 mL) was added N-methylmorpholine (5.7 mL, 51.5 mmole) and this mixture cooled to 0 C. (ice-bath) under anhydrous N2(g). Methyl chloroformate (4.8 mL, 61.8 mmole) was added slowly with stirring under anhydrous conditions, and the reaction allowed to stir at 0 C. for 30 min. and at room temperature for 30 min. The reaction mixture was filtered through a Buchner funnel and the white precipitate washed with ethyl acetate (100 mL). The combined filtrate was extracted with ice-water (1*100 mL) and brine solution (1*100 mL) and then dried over anhydrous magnesium sulfate. The product was filtered and evaporated to a clear oil that was co-evaporated with dry toluene (2*25 mL) and dried in vacuo under high vacuum overnight. The resulting clear oil was crystallized by trituration from anhydrous diethylether (50 mL) to give an off-white solid (2.77 g, 35%) homogeneous by t.l.c. (irrigant=9:1 dichloromethane:methanol, Rf=0.62).

541-59-3 Maleimide 10935, apyrrolines compound, is more and more widely used in various fields.

Reference£º
Patent; Marker Gene Technologies, Inc.; Naleway, John Joseph; Harlan, Fiona Karen; Lusk, Jason Scott; (72 pag.)US2018/207287; (2018); A1;,
Pyrroline – Wikipedia
1-Pyrroline | C4H7N – PubChem