HRID1724646

反应详情

EQUATION

反应方程式

HRID 1724646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

0.2 g (0.76 mmol) of methyl 2-cyano-3-[(4-methyl-3-pyridinyl)amino]-3-(methylsulfanyl)-2-propenoate are dissolved with 0.13 g (0.85 mmol) of 2-cyclopentylethanamidine hydrochloride and 0.23 g (1.67 mmol) of potassium carbonate in 4 ml of DMF and stirred at 90° C. for 3 days. After cooling, the product is purified by preparative HPLC (YMC Gel ODS-AQ S 5/15 μm; eluent A: water, eluent B: aceto-nitrile; gradient: 0 min 30% B, 5 min 30% B, 50 min 95% B) purified. 60 mg (25% of theory) of the product are obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe product is purified by preparative HPLC (YMC Gel ODS-AQ S 5/15 μm; eluent A: water, eluent B: aceto-nitrile; gradient: 0 min 30% B, 5 min 30% B, 50 min 95% B)
  3. custompurified
  4. custom60 mg (25% of theory) of the product are obtained