HRID490261

反应详情

EQUATION

反应方程式

HRID 490261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-{4-[1-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-quinazolin-2-yl)-2-methyl-propylamino]-3-oxo-butyl}-isoindole-1,3-dione (1.5 g from previous step), triethylamine (245 mg, 2.42 mmol), and p-toluoyl chloride (374 mg, 2,42 mmol) in methylene chloride (10 mL) was stirred at room temperature for 2.0 h. The reaction was washed sequentially with 0.5 N HCl, water, 5% NaHCO3, water, and brine and dried (Na2SO4). The filtrate was concentrated in vacuo and purified by flash chromatography (silica gel 3:2 hexanes:EtOAc as eluent) to provide the title compound as a white solid (0.7 g, 35%, 2 steps). MS(ES+) m/e 675 [M+H]+.

WORKUP

后处理

  1. washThe reaction was washed sequentially with 0.5 N HCl, water, 5% NaHCO3, water, and brine
  2. dry with materialdried (Na2SO4)
  3. concentrationThe filtrate was concentrated in vacuo
  4. custompurified by flash chromatography (silica gel 3:2 hexanes:EtOAc as eluent)