HRID572928
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 2-(3-cyanophenyl)acetic acid (1, 6.2 mmol) in methanol (20 ml) was added sulfurous dichloride (5 ml) and 0.1 ml N,N-dimethylformamide. Then the reaction mixture was heated to 80° C. for 2 h. When TLC indicated that the starting material was consumed, the mixture was concentrated to give the residue. The residue was poured into water (20 ml) and was extracted by ethyl acetate (50 m1*2). The organic layer was dried by anhydrous sodium sulfate, filtered, concentrated to give the desired product. LC-MS: m/z (M+H)=176.5
WORKUP
后处理
- customwas consumed
- concentrationthe mixture was concentrated
- customto give the residue
- extractionwas extracted by ethyl acetate (50 m1*2)
- dry with materialThe organic layer was dried by anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated