Hydrochloric Acid → HCID 13488878, compound

Participants

Reaction Steps

1.6 g of ethyl 3-{4-[2-(6-acetoxy-2,5,7,8-tetramethylchroman-2-yl)ethoxy]phenyl}-2-chloropropionate, 300 mg of thiourea and 2 ml of sulfolane were heated at 110°-115° C. for 3 hours under a nitrogen stream. A mixture of 4 ml of water, 2 ml of ethylene glycol monomethyl ether and 1 ml of concentrated hydrochloric acid was then added and the whole mixture was heated at 95°-97° C. for 4.5 hours. The mixture was then treated as described in Example 1(a), except that the crude product, in the form of an oil, was purified by column chromatography through silica gel, eluted with a 10:1 by volume mixture of benzene and ethyl acetate, to give the title compound, melting at 152°-154° C.

Provenance & Evidence