HRID620166
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
Boron tribromide (8.9 ml) in dichloromethane (25 ml) was added dropwise, under nitrogen, to a stirred solution of 4-methoxymethyl-5-methyl-6-piperidinopyrimidine (5 g) in dichloromethane (100 ml) at 0°-5°. After a further 2 hours the mixture was poured onto ice, the pH raised to 13 (NaOH) and extracted with chloroform. Extracts were dried (K2CO3) and stripped to a residue, which was triturated with diethyl ether to give 4-hydroxymethyl-5-methyl-6-piperidinopyrimidine, 3.80 g, as a crystalline solid, m.p. 79°-81°.
WORKUP
后处理
- additionAfter a further 2 hours the mixture was poured onto ice
- extractionextracted with chloroform
- dry with materialExtracts were dried (K2CO3)
- customwas triturated with diethyl ether