HRID1755989

反应详情

EQUATION

反应方程式

HRID 1755989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of 1-ethoxy-1-(4-ethoxypyrimidin-2-yl)-ethylene (2.7 g) in acetone (20 ml) was treated with hydrochloric acid (6 ml of a 2M solution). The reaction mixture was allowed to stand for 16 hours, then warmed at 40° C. for 11/2 hours, and concentrated. The residue was diluted with water and neutralised with sodium bicarbonate. The aqueous phase was extracted with ethyl acetate (×2) and the combined extracts were washed with brine, dried and concentrated to give 2-acetyl-4-ethoxypyrimidine (1.8 g, 78% yield) as a colourless oil which partially solidified on standing, and was used without further purification; IR maximum (film): 1717cm-1 ; 1H NMR (270 MHz): δ1.45(3H,t), 2.74(3H,s), 4.53(2H,q), 6.85(1H,d), 8.60(1H,d) ppm.

WORKUP

后处理

  1. concentrationconcentrated
  2. additionThe residue was diluted with water and neutralised with sodium bicarbonate
  3. extractionThe aqueous phase was extracted with ethyl acetate (×2)
  4. washthe combined extracts were washed with brine
  5. customdried
  6. concentrationconcentrated