HRID894092

反应详情

EQUATION

反应方程式

HRID 894092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.3 g of mercury oxide is added to 0.3 g of N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-cyclohexyl-thiourea (melting point 194°-196° C., prepared from 4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonamide and cyclohexyl mustard oil) in a mixture of 50 ml of water and 50 ml of methanol and the whole is stirred for 3 hours at 40°-45° C. The precipitated mercury sulfide is filtered off with suction, the filtrate is concentrated under reduced pressure, the residue is treated with very dilute ammonia, filtered and the filtrate is acidified with dilute hydrochloric acid. The precipitated N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-2,5-cyclohexyl-urea is recrystallized from dilute acetone and melts at 211°-213° C. The mixed melting point with the compound obtained according to Example 1 is without depression.

WORKUP

后处理

  1. filtrationThe precipitated mercury sulfide is filtered off with suction
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. additionthe residue is treated with very dilute ammonia
  4. filtrationfiltered
  5. customThe precipitated N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-2,5-cyclohexyl-urea is recrystallized from dilute acetone and melts at 211°-213° C
  6. customThe mixed melting point with the compound obtained