HRID1755990

反应详情

EQUATION

反应方程式

HRID 1755990 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-acetyl-4-ethoxypyrimidine (1.8 g), hydroxylamine hydrochloride (0.83 g) and sodium acetate (2.2 g) in a mixture of ethanol:water (30:10 ml) was heated under reflux for 3 hours. The reaction mixture was then poured into water and extracted with ethyl acetate (×3). the combined extracts were washed with brine, dried and concentrated to give a solid which was washed with hexane to give (E)-2-acetyl-4-ethoxypyrimidine oxime as an off-white solid (1.15 g, 60% yield); 1H NMR (270 MHz): δ1.44(3H,t), 2.38(3H,s), 4.50(2H,q), 6.68(1H,d), 8.48(1H,d), 9.80(1H,brs) ppm.

WORKUP

后处理

  1. temperatureunder reflux for 3 hours
  2. extractionextracted with ethyl acetate (×3)
  3. washthe combined extracts were washed with brine
  4. customdried
  5. concentrationconcentrated
  6. customto give a solid which
  7. washwas washed with hexane