HRID620159
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
A solution of boron tribromide (9.02 ml) in dichloromethane (100 ml) was added dropwise to a stirred solution of 2-methoxymethyl-4-morpholinopyrimidine (4.99 g) in dichloromethane (50 ml) at -25° under nitrogen. After 15 minutes the mixture was allowed to warm to 0°-5°, and left to stand for 2 hours at this temperature. After pouring onto ice, the pH was raised to 14 (NaOH), and the organic phase separated off. The aqueous phase was further extracted with chloroform, and the combined extracts dried (K2CO3) and stripped. The residue was triturated with ether to give 2-hydroxymethyl-4-morpholinopyrimidine (3.16 g) as a crystalline solid, m.p. 76°-8°.
WORKUP
后处理
- temperatureto warm to 0°-5°
- waitleft
- waitto stand for 2 hours at this temperature
- additionAfter pouring onto ice
- customthe organic phase separated off
- extractionThe aqueous phase was further extracted with chloroform
- dry with materialthe combined extracts dried (K2CO3)
- customThe residue was triturated with ether