HRID414758

反应详情

EQUATION

反应方程式

HRID 414758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 27.4 g of 2-methyl-4-amino-5-formylpyrimidine and 1000 ml of methanol was added, while stirring at room temperature, dropwise gradually 25 ml of an aqueous solution containing 15.2 g of hydroxylamine hydrochloride. The reaction was allowed to proceed for further 3 hours at room temperature, which was then concentrated to dryness under reduced pressure. The concentrate was recrystallized from ethanol to give 25.6 g of 2-methyl-4-amino-5-pyrimidine aldoxime hydrochloride. The resulting mother liquor was concentrated to dryness under reduced pressure, followed by subjecting the concentrate to crystallization from a mixture of methanol/ether (1:1 V/V) to give 10.8 g of 2-methyl-4-amino-5-pyrimidine aldoxime hydrochloride. The total yield was 96.5%.

WORKUP

后处理

  1. additionwas added
  2. concentrationwhich was then concentrated to dryness under reduced pressure
  3. customThe concentrate was recrystallized from ethanol