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
Thionyl chloride (0.18 mL, 2.4 mmol) was added to a suspension of 2-acetylamino-4-hydroxymethylpyrimidine (290 mg, 1.7 mmol, Reference Compound No. 4-3) in anhydrous methylene chloride (10 mL) at room temperature, and the mixture was stirred for 30 minutes. The solvent was evaporated under reduced pressure, then water (50 mL) and ethyl acetate (100 mL) were added thereto and the mixture was separated into the organic layer and the aqueous layer, and the aqueous layer was extracted twice with ethyl acetate (50 mL). The whole organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give 68 mg of the title Reference Compound as a yellow solid (Yield: 18%).
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- additionwater (50 mL) and ethyl acetate (100 mL) were added
- customthe mixture was separated into the organic layer
- extractionthe aqueous layer, and the aqueous layer was extracted twice with ethyl acetate (50 mL)
- dry with materialThe whole organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure