Acetone → 4-amino-5-chloro-2-[2-(methylsulfinyl)ethoxy]-N-[2-(diethylamino)ethyl]benzamide hydrochloride monohydrate

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-amino-5-chloro-2[2-(methylsulfinyl)ethoxy]-N-[2-(diethylamino)ethyl]benzamide (84.50 g, 22.5 mmoles), acetone (592 ml) and 2-propanol (169 ml) was stirred and warmed until complete solution (ca. 25° C.) and then 56.2 ml of 4N HCl (1 equivalent) was all at once. The temperature rose to 32° C. After one hour at ambient temperature the mixture was stored at 0° C. for 18 hours. The hydrochloride salt was collected by filtration, rinses with acetone and dried in vacuo over P2O5 for six hours. Yield: 89.6 g (96.6%); mp 117°-124° C.

Provenance & Evidence