HRID1978573

反应详情

EQUATION

反应方程式

HRID 1978573 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of methyl 7-(4-chlorophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.95 g) in 1,2-dimethoxyethane (50 ml) was added 6N hydrochloric acid (30 ml), and the mixture was stirred at 70° C. for 64 hours. The mixture was cooled to room temperature, extracted with ethylacetate, saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. Precipitated crystals were collected by filtration, and the crystals was washed with diisopropylether and hexane to give pale yellow crystals of 7-(4-chlorophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (804.9 mg).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with ethylacetate, saturated brine
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customPrecipitated crystals
  6. filtrationwere collected by filtration
  7. washthe crystals was washed with diisopropylether and hexane