反应详情

To cold (−20° C.) and dry methanol (195 ml) was added dropwise thionylchloride (28 ml). H—D—Cha—OH.HCl (40 g) was added and the reaction mixture was heated under reflux for 5 hours The mixture was concentrated in vacuo and coevaporated with methanol (3 times). The residue was crystallized from methanol/diethyl ether yielding H—D—Cha—OMe.HCl as a white crystalline powder (40.9 g). TLC: Rf=0.66, silica gel, n-butanol/acetic acid/water 10/1/3 v/v/v.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 5 hours The mixture
3. concentrationwas concentrated in vacuo
4. customThe residue was crystallized from methanol/diethyl ether