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

Participants

Reaction Steps

1-(3-Chloropropyl)pyrrolidine oxalate (134.8 kg) was suspended in water (226 l) and methyl tert-butyl ether (83.4 kg) added. The stirred mixture was basified to pH>11 by addition of 49% w/w aqueous potassium hydroxide solution (138.9 kg). A line wash of water (22.6 l) was applied. The lower aqueous layer was separated and transferred to a second reactor. The upper organic layer was transferred to 200 l drums. A line wash of methyl tert-butyl ether (16.7 kg) was applied. The aqueous layer was recharged to the original reactor and further extracted with methyl tert-butyl ether (83.4 kg). The lower aqueous layer was discarded. The original organic layer was recharged from the drums. A line wash of methyl tert-butyl ether (16.7 kg) was applied. The combined organic layers were washed with 23% w/w aqueous potassium chloride solution (64.8 kg) to give a solution of 1-(3-chloropropyl)pyrrolidine (83.9 kg) in methyl tert-butyl ether. The required amount of solution can then be used as appropriate.

Provenance & Evidence