HRID1067254

反应详情

EQUATION

反应方程式

HRID 1067254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of N-(4-chlorobenzyl)-4-hydroxy-6-(hydroxymethyl)-3-quinolinecarboxamide from Preparation No. 3 (300 mg,), K2CO3 (485.1 mg), and CH3I (0.11 mL) in 4 mL anhydrous DMF is heated at 90° C. for 3 hours. The reaction is cooled to room temperature and diluted with H2O to dissolve any salts and precipitate the product. The crude product is adsorbed onto silica and chromatographed eluting with 3% MeOH in CH2Cl2. Fractions homogenous by TLC are combined and condensed to afford 154.2 mg (49%) of the title compound as a white solid.

WORKUP

后处理

  1. dissolutionto dissolve any salts
  2. customprecipitate the product
  3. customchromatographed
  4. washeluting with 3% MeOH in CH2Cl2
  5. customcondensed