HRID343272

反应详情

EQUATION

反应方程式

HRID 343272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound and its preparation has been described in Great Britain Patents 1,390,014 and 1,390,015. Piperazine hexahydrate (194 g, 1 mole) was dissolved in 250 ml H2O. The solution was acidified to pH 4.5 with 6N HCl. Furoyl chloride (130.5 g, 1 mole, Aldrich) was added along with 10% NaOH solution at such a rate that the pH was maintained at 4.5. After 1 hour, the solution was made basic (pH=8.5) with NaOH solution. The reaction mixture was continuously extracted with chloroform for 36 hours. The CHCl3 extract was dried over MgSO4, and filtered. Distillation gave 108.2 g product (60%), b.p. 132°-138° C./0.6 mm Hg, m.p. 69°-70° C.

WORKUP

后处理

  1. customThis compound and its preparation
  2. temperaturewas maintained at 4.5
  3. extractionThe reaction mixture was continuously extracted with chloroform for 36 hours
  4. extractionThe CHCl3 extract
  5. dry with materialwas dried over MgSO4
  6. filtrationfiltered
  7. distillationDistillation