HRID1949151

反应详情

EQUATION

反应方程式

HRID 1949151 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

600 mg (26.1 mmol) sodium were added slowly to MeOH (500 ml). Then a solution of 1.16 g (3.0 mmol) 3-[[3-[oxo-(2-thienylmethylamino)methyl]-2-quinolyl]-thio]propanoic acid methyl ester (Example 2) in MeOH (60 ml) was added at RT. Then the reaction solution was heated for 1 h at 70° C. After cooling to RT the mixture was concentrated to small volume under vacuum. The residue was taken up with water and the solution was washed with EE. Then it was acidified with concentrated hydrochloric acid to pH 3. The deposit formed was filtered off and dried. 805 mg (2.7 mmol, 90%) 2-mercapto-N-(thiophen-2-ylmethyl)quinoline-3-carboxamide were obtained.

WORKUP

后处理

  1. temperatureAfter cooling to RT the mixture
  2. concentrationwas concentrated to small volume under vacuum
  3. washthe solution was washed with EE
  4. customThe deposit formed
  5. filtrationwas filtered off
  6. customdried