HRID1013868
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 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug, Column chromatography of the plug with hexane:acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid.
WORKUP
后处理
- temperatureThe resulting mixture was refluxed for 2 h
- customthe solvent was removed under reduced pressure
- customto afford a dark residue
- customThe solvent was evaporated
- customto afford a plug, Column chromatography of the plug with hexane