反应详情

Thionyl chloride (17.7 mL, 0.24 mol) in methylene chloride (40 mL) was added dropwise to a solution of N'-hydroxy-2-(3,4-dimethylphenyl)ethanimidamide (10.8 g, 0.06 mol), methylene chloride (130 mL) and pyridine (9.8 mL, 0.12 mol) at 5° C. After 3 hours, the mixture was poured into water and the organic layer separated. The organic layer was washed with saturated aqueous sodium chloride, dried over magnesium sulfate and concentrated in vacuo. Recrystallization from ethyl ether afforded the desired product (4.3 g, 32%) as an off-white solid, m.p. 127°-130° C.

1. customthe organic layer separated
2. washThe organic layer was washed with saturated aqueous sodium chloride
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customRecrystallization from ethyl ether