Methanol → HCID 87158563, compound

Participants

Reaction Steps

1-Benzyl-3-(3,5-dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidine (3.7 g) was dissolved in 1,2-dichloroethane (20 ml), added with 1-chloroethyl chloroformate (2.7 g) at room temperature, and then refluxed under heating for 3 hours. The reaction solution was concentrated under reduced pressure, and the residue obtained was added with methanol (30 ml) and further refluxed under heating for 2 hours. The reaction solution was concentrated under reduced pressure and the residue obtained was added with t-butyl methyl ether and water to separate the aqueous layer. After that, the organic layer was again washed with a 1 M aqueous solution of hydrochloric acid, and the aqueous layers were combined, added with a saturated aqueous solution of potassium carbonate to make the liquid alkaline, and extracted with t-butyl methyl ether. The aqueous phase was extracted again with t-butyl methyl ether, and the organic layers were combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure to obtain 3-(3,5-dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidine (2.6 g).

Provenance & Evidence