HRID524391

反应详情

EQUATION

反应方程式

HRID 524391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

Methyl 2-(4-chlorosulfonylphenyl)acetate (2.0 g, 8.04 mmol) was taken in dry DCM (50 mL) under argon atmosphere and cooled to 0-5° C., morpholine (0.77 mL, 8.84 mmol) followed by triethylamine (1.16 mL, 8.84 mmol) was added dropwise to the mixture at 0-5° C. Reaction mixture was then brought to room temperature and stirred for additional 2 hours. Reaction mixture was washed with water followed by brine solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the crude product, which was purified by column chromatography using 14-20% ethyl acetate in hexane as eluent to give Methyl 2-(4-morpholinosulfonylphenyl)acetate (1.5 g).

WORKUP

后处理

  1. additionwas added dropwise to the mixture at 0-5° C
  2. customReaction mixture
  3. customwas then brought to room temperature
  4. customReaction mixture
  5. washwas washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto give the crude product, which
  9. customwas purified by column chromatography