反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a stirred anhydrous benzyl alcohol (80 ml), was added pieces of sodium metal (1.73 g, 75 mmol). After the reaction completed, the mixture was cooled in an ice bath and 5-tert-Butyl-2,4,6-trichloro-pyrimidine (9 g, 37.5 mmol) was added. After 1 hr., the mixture was stirred at room temperature for overnight and evaporated in vacuo. The residue was dissolved in ethyl acetate, washed with water, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The crude product was purified by silica gel column chromatography (eluent, ether:hexanes (1:19)) to afford 13 g (90%) of a white solid. m.p. 96° C.; 1H NMR (200 MHz, CDCl3) δ 1.50 (9H, s), 5.37 (2H, s), 5.41 (2H, s), 7.34-7.46 (10H, m).
WORKUP
后处理
- temperaturethe mixture was cooled in an ice bath
- customevaporated in vacuo
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water
- dry with materialdried with anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
- customThe crude product was purified by silica gel column chromatography (eluent, ether:hexanes (1:19))