chloroform methanol HOAc → HCID 131715558, compound

Participants

Reaction Steps

A stirred solution of (cis)-3-hydroxy-1-[2-(1-pyrrolidinyl)ethyl]-1,3,4,5-tetrahydro-4-(4-methoxyphenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one, monohydrochloride (3.3 g, 0.0056 mmol) in 80 ml of acetic anhydride under argon was heated in an oil bath at 114°-119° C. for 4.5 hours. The bulk of acetic anhydride was removed on a rotary evaporator at 0.2 mm and the solid residue (12 g) was suspended in 30 ml of ethyl acetate, diluted with 60 ml of ether, cooled for 1 hour, filtered, washed with ether, and dried in vacuo overnight; yield, 2.60 g; melting point 228°-230° C. (dec.); s, 225° C. TLC: Rf =0.48 (8:1:1, chloroform-methanol-acetic acid).

Provenance & Evidence