HRID2284894
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2,4,5-trichloropyrimidine (5 g, 27.32 mmol) in THF:water (1:1, 40 mL), was added sodium thiomethoxide (2.15 g, 30.01 mmol) at 0° C., and the mixture was stirred at rt for 4 h. TLC showed completion of starting material and formation of a slightly polar spot (TLC system: hexane charred in iodine). The reaction mixture was concentrated, water (20 ml) was added, and the product was extracted with ethyl acetate (2×20 ml). The organic layer was dried over sodium sulfate and concentrated to afford the desired compound as a white solid (5 g, 94.8%). MS m/z: 195.2 (ES+, M+H).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additionwater (20 ml) was added
- extractionthe product was extracted with ethyl acetate (2×20 ml)
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated