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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 h. The mixture was concentrated in vacuo and coevaporated with methanol (3 times). The residue was crystallized from methanoldiethylether yielding H-D-Cha-OMe.HCl as a white crystalline powder (40.9 g),

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 5 h
3. concentrationThe mixture was concentrated in vacuo
4. customThe residue was crystallized from methanoldiethylether