HRID51842
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred suspension of 2.00 g (5.36 mmol) 1-benzoyl-3-{2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea in 13 ml methanol was added dropwise 0.15 ml (0.80 mmol) 5.4 M sodium methylate solution and stirring continued for 1 h at room temperature. The mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Flash chromatography (ethyl acetate) afforded 1.40 g (97%) {2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea as an amber oil. ES-MS m/e (%): 270 (M+H+, 100).
WORKUP
后处理
- additionThe mixture was then poured onto water
- extractionextracted three times with ethyl acetate
- dry with materialThe combined organic phases were dried over sodium sulfate
- concentrationconcentrated in vacuo