HRID2248562

反应详情

EQUATION

反应方程式

HRID 2248562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.4 g of 4-dimethylaminobenzenesulphonyl chloride (Chem. Ber. 43, 3038, (1910)) are added to a solution comprising 2.34 g of 5-aminovaleric acid and 2.4 g of sodium hydroxide dissolved in 24 cm3 of water, followed by the addition of 24 cm3 of tetrahydrofuran in order to obtain a solution. The temperature rises to 36° C. The mixture is kept stirring for 4 hours, the tetrahydrofuran is evaporated off, the reaction medium is acidified using acetic acid and extracted with chloroform, the organic phase is dried and the solvents are removed under reduced pressure. 3.7 g of expected product are obtained. M.p. 105°-110° C. After crystallization in an isopropanol/water mixture (1:1), the product, melting point 118°-120° C., is obtained.

WORKUP

后处理

  1. customto obtain a solution
  2. customrises to 36° C
  3. customthe tetrahydrofuran is evaporated off
  4. extractionextracted with chloroform
  5. customthe organic phase is dried
  6. customthe solvents are removed under reduced pressure