HRID1815175
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 6-chloro-pyrimidine-4-carbonitrile (1.37 g, 9.84 mmol) stirring in 10 ml THF under N2 was added a methylamine solution (2.0 M in THF, Aldrich) in aliquots, causing immediate precipitation. Reaction progress was monitored after addition of 5 ml methylamine solution, then 3 ml, then 2 ml. The mixture was concentrated and filtered through a pad of silica, eluting with 2%->5% MeOH in CH2Cl2 to obtain 6-methylamino-pyrimidine-4-carbonitrile as a pale yellow solid. MS: 135.0 (M+1); Calc'd. for C6H6N4—134.14.
WORKUP
后处理
- customprecipitation
- customReaction progress
- concentrationThe mixture was concentrated
- filtrationfiltered through a pad of silica
- washeluting with 2%->5% MeOH in CH2Cl2