HRID426220
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 mixture of 2,4-dichloro-6-methylpyrimidine (12.5 g, 76.65 mmol), N-chloro succinimide (12.28 g, 92 mmol), and benzoyl peroxide (2.78 g, 11.5 mmol) in carbon tetrachloride (150 ml) was refluxed for 24 hr. After cooling to room temperature, the mixture was filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, from hexane to 2% ether in hexane) to afford 6 g (40%) of 2,4-dichloro-6-chloromethyl-pyrimidine as a white solid. 1H NMR (200 MHz, CDCl3) δ 4.58 (2H, s), 7.55 (1H, s).
WORKUP
后处理
- temperaturewas refluxed for 24 hr
- filtrationthe mixture was filtered
- customevaporated in vacuo
- customThe residue was purified by silica gel column chromatography (eluent, from hexane to 2% ether in hexane)