Sodium Hydroxide → 1-(3-Chloropropyl)-pyrrolidine

A 71.5% w/w aqueous solution of 1-(3-chloropropyl)pyrrolidine hydrochloride (25 kg) was diluted with water (14 l) and methyl tert-butyl ether (12 l) added. The stirred mixture was basified to pH>11 by addition of 46% w/w aqueous sodium hydroxide solution (6.5 l). The layers were separated and he lower aqueous phase was further extracted with methyl tert-butyl ether (12 l). The combined organic layers were washed with 20% w/w aqueous sodium chloride solution (12.5 kg) to give a solution of 1-(3-chloropropyl)pyrrolidine in methyl tert-butyl ether.

1. additionadded
2. customThe layers were separated
3. extractionhe lower aqueous phase was further extracted with methyl tert-butyl ether (12 l)
4. washThe combined organic layers were washed with 20% w/w aqueous sodium chloride solution (12.5 kg)

ORD record

ord-10963a4f32404356aa7ff3d2deb5fc9d

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08754240B2