HRID524342

反应详情

EQUATION

反应方程式

HRID 524342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 6-methyl-4-oxo-5-(3-trifluoromethyl-phenyl)-1,4-dihydro-pyridine-3-carboxylic acid 4-methanesulfonyl-benzylamide (preparation 1, 100 mg, 0.215 mmol), K2CO3 (48 mg, 0.344 mmol) and iodoethane (20 μL, 0.250 mmol) in DMF (1 mL) is stirred for 30 min at 80° C. (microwave). The reaction mixture is diluted with MeOH, filtered and purified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.3% NH4OH, 60° C.). Yield: 52 mg (49% of theory); ESI mass spectrum: [M+H]+=493; Retention time HPLC: 1.03 min (Z003_001).

WORKUP

后处理

  1. filtrationfiltered
  2. custompurified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.3% NH4OH, 60° C.)
  3. custom1.03 min (Z003_001)