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
Trityl chloride (9.43 g) is added in one portion to a solution of 2-hydroxymethyl-5-methoxy-4-pyridone (5 g) and 4-dimethylaminopyridine (4.2 g) in dry dimethylformamide (80 mL) and the solution stirred at room temperature for 12 hours. The mixture is then heated on a steam bath for 3 hours and diluted with iced water (300 mL) to give a light brown solid. The solid is collected, washed with water and sucked dry. The solid is dissolved in hot ethyl acetate to give a clear solution which immediately deposits a granular off-white solid. The solid does not redissolve on further heating. After cooling the solid is collected, washed with ethyl acetate and diethyl ether and dried to give 5-methoxy-2-trityloxymethyl-4-pyridone (7.5 g) as an off-white solid, m.p. 185–7° C.
WORKUP
后处理
- temperatureThe mixture is then heated on a steam bath for 3 hours
- customto give a light brown solid
- customThe solid is collected
- washwashed with water
- customsucked dry
- dissolutionThe solid is dissolved in hot ethyl acetate
- customto give a clear solution which
- dissolutionThe solid does not redissolve on further heating
- temperatureAfter cooling the solid
- customis collected
- washwashed with ethyl acetate and diethyl ether
- customdried