HRID1978587

反应详情

EQUATION

反应方程式

HRID 1978587 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 methyl 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) was added 6N hydrochloric acid (60 ml), and the mixture was stirred at 70° C. for 5 hours and concentrated under reduced pressure. To the residue was added ethanol, and to the mixture were added 8N sodium hydroxide solution and 1N sodium hydroxide solution to make the solution pH 6-7. The mixture was concentrated under reduced pressure to give solid, which was collected by filtration and washed with water, 2-propanol, acetone and diisopropylether to give yellow powder of 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (549.5 mg).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added ethanol
  3. additionto the mixture were added 8N sodium hydroxide solution and 1N sodium hydroxide solution
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customto give solid, which
  6. filtrationwas collected by filtration
  7. washwashed with water, 2-propanol, acetone and diisopropylether