HRID1580687

反应详情

EQUATION

反应方程式

HRID 1580687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7.8 Grams of 4-(7-Chloro-4-quinolylamino)-benzenesulphonyl chloride hydrochloride [prepared as in Example 1(b)] were added in portions to a stirred ice-cooled mixture of 3.63 grams of 4-amino-1-cyclohexyl-piperidine and 21.2 grams of sodium carbonate in 60 milliliters of water and 50 milliliters of chloroform. After stirring overnight at room temperature the chloroform layer was separated, washed with water, dried and evaporated to give a brown solid. This was triturated with hexane, the resultant solid dissolved in chloroform and diiso-propyl ether added to precipitate a solid which was triturated with hexane to give 1.9 grams of the title compound as the hemihydrate. Melting point 192°-193°C.

WORKUP

后处理

  1. temperaturecooled
  2. customwas separated
  3. washwashed with water
  4. customdried
  5. customevaporated
  6. customto give a brown solid
  7. customThis was triturated with hexane
  8. dissolutionthe resultant solid dissolved in chloroform
  9. additiondiiso-propyl ether added
  10. customto precipitate a solid which
  11. customwas triturated with hexane