HRID745173

反应详情

EQUATION

反应方程式

HRID 745173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.

WORKUP

后处理

  1. customThe residue obtained
  2. extractionthe chloroform layer was extracted with water
  3. dry with materialThe chloroform layer was dried
  4. filtrationfiltered
  5. customsolvent removed
  6. customto give a dark brown oil
  7. customThis salt was recrystallized from methanol-diethyl ether
  8. customdried in vacuo overnight at 80° C