HRID21486

反应详情

EQUATION

反应方程式

HRID 21486 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Fluoro-4-chloro-5-methoxycarbonyloxyaniline (2.00 g, 6.86 mmol), potassium carbonate (1.42 g, 10.3 mmol), benzyl chloroformate (1.17 g, 6.86 mmol) and acetone (20 ml) as a solvent were charged into a 100 cc two-necked flask, and heated for 2 hours while refluxing. After completion of the reaction, the mixture was added to 1H hydrochloric acid (50 ml), and extracted with ethyl acetate (50 ml×3). After drying, the organic layer was concentrated to obtain substantially pure benzyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate as a solid (2.21 g, 91.1% yield).

WORKUP

后处理

  1. temperatureheated for 2 hours
  2. temperaturewhile refluxing
  3. customAfter completion of the reaction
  4. extractionextracted with ethyl acetate (50 ml×3)
  5. customAfter drying
  6. concentrationthe organic layer was concentrated