HRID1978575

反应详情

EQUATION

反应方程式

HRID 1978575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 7-(4-fluorophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.55 g) in 1,2-dimethoxyethane (20 ml) was added 6N hydrochloric acid (10 ml), and the mixture was refluxed for 29 hours, cooled to room temperature, extracted with ethyl acetate, saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give crystals, which were collected by filtration. The crystals were washed with diisopropylether and hexane to give pale yellow crystals of 7-(4-fluorophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (490.7 mg).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 29 hours
  2. extractionextracted with ethyl acetate, saturated brine
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give crystals, which
  6. filtrationwere collected by filtration
  7. washThe crystals were washed with diisopropylether and hexane