Thionyl Chloride → HCID 15052150, compound

Participants

Reaction Steps

0.14 ml of thionyl chloride was added to a solution of 329 mg of the product of Step C in 3.3 ml of methylene chloride and the mixture was stirred for 15 minutes at ambient temperature, then evaporated to dryness under reduced pressure. The residue was taken up in 25 ml of ether at reflux, treated with activated charcoal, filtered and concentrated to 7 ml. After separation, 300 mg of the expected product melting at approx. 70° C. were obtained which was used as is for Step E. An analytical sample was prepared by dissolving 300 mg of the product in 10 ml of hot methyl ethyl ketone which was concentrated to 2 ml, then adding 2 ml of pentane. After separating, 65 mg of the desired product melting at approx. 70° C. were obtained.

Provenance & Evidence