HRID1287792

反应详情

EQUATION

反应方程式

HRID 1287792 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-(β-phenylethylamino)-5-sulphamyl-benzoic acid (3.35 g), benzyl bromide (5.3 g), and anhydrous ethanol (30 ml) was refluxed for 48 hours. After cooling, the precipitated ethyl ester was collected by suction, recrystallized from ethanol and saponified by heating in 1N sodium hydroxide (30 ml) for 1 hour. The 3-benzylamino-4-(β-phenylethylamino)-5-sulphamyl-benzoic acid was precipitated at room temperature by addition of 4N hydrochloric acid until the pH was 2.5. After recrystallization from aqueous ethanol, the compound was obtained with a melting point of 203° C.

WORKUP

后处理

  1. temperaturewas refluxed for 48 hours
  2. temperatureAfter cooling
  3. customthe precipitated ethyl ester was collected by suction
  4. customrecrystallized from ethanol
  5. temperaturesaponified by heating in 1N sodium hydroxide (30 ml) for 1 hour
  6. customThe 3-benzylamino-4-(β-phenylethylamino)-5-sulphamyl-benzoic acid was precipitated at room temperature by addition of 4N hydrochloric acid until the pH was 2.5
  7. customAfter recrystallization from aqueous ethanol
  8. customthe compound was obtained with a melting point of 203° C.