HRID1906150

反应详情

EQUATION

反应方程式

HRID 1906150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-chloropyrimidin-2-one (587 mg) and crude 3-bromoacetylfuran (2.00 g, ca. 4.5 mmol, based on purity ca. 40% by 1H n.m.r; contaminated with 3-dibromoacetylfuran and diethyl ether) in triethylamine (0.95 ml) and ethanol (25 ml) was stirred at room temperature. After 45 min with solvent was removed and the residue triturated with ethyl acetate. The resulting solid was collected and retriturated with water. This gave a buff solid which was crystallised from ethyl acetate to give the title pyrimidinone (335 mg), m.p. 195°-197° C. (dec), λmax (EtOH) 333 nm (ε 2,530).

WORKUP

后处理

  1. customAfter 45 min with solvent was removed
  2. customthe residue triturated with ethyl acetate
  3. customThe resulting solid was collected
  4. customretriturated with water
  5. customThis gave a buff solid which
  6. customwas crystallised from ethyl acetate