HRID918681

反应详情

EQUATION

反应方程式

HRID 918681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-amino-4-isopropylamino-5-sulphamyl-benzoic acid (2.62 g), benzyl bromide (4.28 g), and anhydrous ethanol (25 ml) was refluxed for 24 hours. The reaction mixture was evaporated in vacuo. 1N sodium hydroxide (30 ml) was added, and the mixture was heated on a steam bath for 1 hour. After cooling and extracting with diethyl ether, the aqueous layer was adjusted to a pH of 3 by addition of 4N hydrochloric acid. The precipitated 3-benzylamino-4-isopropylamino-5-sulphamyl-benzoic acid was collected by suction and recrystallized from aqueous ethanol. The melting point was 233°-234°C.

WORKUP

后处理

  1. temperaturewas refluxed for 24 hours
  2. customThe reaction mixture was evaporated in vacuo
  3. addition1N sodium hydroxide (30 ml) was added
  4. temperaturethe mixture was heated on a steam bath for 1 hour
  5. temperatureAfter cooling
  6. extractionextracting with diethyl ether
  7. additionthe aqueous layer was adjusted to a pH of 3 by addition of 4N hydrochloric acid
  8. customThe precipitated 3-benzylamino-4-isopropylamino-5-sulphamyl-benzoic acid was collected by suction
  9. customrecrystallized from aqueous ethanol