HRID490248

反应详情

EQUATION

反应方程式

HRID 490248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

To a solution of 2-(1-amino-2-methyl-propyl)-3-benzyl-7-chloro-3H-quinazolin-4-one (1.87 g, 5.48 mmol) in DMF (30 mL) was added bromoacetaldehyde dimethylacetal (2.78 g, 16.44 mmol) and potassium carbonate (2.27 g, 16.44 mmol) and the resulting suspension was heated at 135° C. for 18 h. The cooled reaction was concentrated in vacuo, triturated with methylene chloride to remove any solids, and the filtrate was concentrated in vacuo. The residue was purified by flash chromatography (silica gel; 2:1 hexanes:ethyl acetate) to give the title compound as a pale yellow oil (1.38 g, 59%). MS(ES+) m/e 430 [M+H]+.

WORKUP

后处理

  1. customThe cooled reaction
  2. concentrationwas concentrated in vacuo
  3. customtriturated with methylene chloride
  4. customto remove any solids
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was purified by flash chromatography (silica gel; 2:1 hexanes:ethyl acetate)