HRID1788752

反应详情

EQUATION

反应方程式

HRID 1788752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1,4-dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester (4.0 g, 12.0 mmol; see Example 1A) in dry dimethylformamide (10 ml) was treated with finely ground potassium carbonate (6.6 g, 48.0 mmoles) and allyl bromide (1.7 ml, 20.0 mmole). The resulting suspension was allowed to stir under argon at room temperature for 10 hours. The reaction was diluted with ethyl acetate, filtered and the filtrate was washed with water and brine. It was dried over anhydrous magnesium sulfate and evaporated to provide a yellow oil. Purification by flash chromatography (20% ethyl acetate in hexanes) yielded the title compound (2.64 g) as a yellow oil.

WORKUP

后处理

  1. filtrationfiltered
  2. washthe filtrate was washed with water and brine
  3. dry with materialIt was dried over anhydrous magnesium sulfate
  4. customevaporated
  5. customto provide a yellow oil
  6. customPurification by flash chromatography (20% ethyl acetate in hexanes)