HRID1801748

反应详情

EQUATION

反应方程式

HRID 1801748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of commercially available 2-amino-5-cyano-pyrimidine [CAS-No. 1753-48-6] (1.39 g, 11.6 mmol), hydroxylamine hydrochloride (1.61 g, 23.2 mol) and potassium carbonate (4.8 g, 34.7 mol) in ethanol (57 ml) was heated under reflux conditions for 3 h. The reaction mixture was evaporated and purified by column chromatography on silica gel (dichloromethane/MeOH 9:1) to yield the title compound (1.28 g, 72%) as an off-white solid. MS (EI) 153.1 [(M)+]; mp 218° C.

WORKUP

后处理

  1. temperaturewas heated under reflux conditions for 3 h
  2. customThe reaction mixture was evaporated
  3. custompurified by column chromatography on silica gel (dichloromethane/MeOH 9:1)