1-Chloroethyl chloroformate → methyl (3R*,4S*)-4-(3,4-dichlorophenyl)pyrrolidine-3-carboxylate monohydrochloride

To a solution of the compound (33.4 g) obtained in step 2 in acetonitrile (250 mL) was added ACE-Cl (13.9 g) at room temperature, and the mixture was stirred at 90° C. for 2 hr. The reaction mixture was cooled, and the solvent was evaporated under reduced pressure. Methanol (250 mL) was added to the residue, and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was cooled, and the solvent was evaporated under reduced pressure to give methyl (3R*,4S*)-4-(3,4-dichlorophenyl)pyrrolidine-3-carboxylate monohydrochloride (26.9 g, 98%) as a pale yellow powder.

1. temperatureThe reaction mixture was cooled
2. customthe solvent was evaporated under reduced pressure
3. additionMethanol (250 mL) was added to the residue
4. stirringthe mixture was stirred at 80° C. for 2 hr
5. temperatureThe reaction mixture was cooled
6. customthe solvent was evaporated under reduced pressure

ORD-Eintrag

ord-b950dd2aa4cf44d0bd0ebbd403c90c9c

Quelldatensatz

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08470816B2