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