Water → HCID 12795109, compound

Participants

Reaction Steps

A solution of potassium hydroxide (2.02 g) in water (1.2 ml.) is added to a solution of 9-cyano-5,6,7,8-tetrahydro-9H-pyrrolo[1,2-a]azepine (1.0 g., 0.006 moles) in ethylene glycol (11 ml.) at 5°. The solution thus obtained is placed in an oil bath at 118° and after 3 hours the cooled solution is poured into water (50 ml.). The aqueous alkaline phase is extracted with ether (20 ml.) the aqueous phase is made acidic to pH-2 with concentrated hydrochloric acid at 5°. The product is extracted into ethyl acetate (4×40 ml.), the extract is washed with water to neutrality, dried and evaporated. Crystallization of the residue from ethyl acetate-ether gave 5,6,7,8-tetrahydro-9H-pyrrolo[1,2,a]azepine-9-carboxylic acid, (92% yield), m.p. 129°-130° C.

Provenance & Evidence