反应 #470443

ord-16e426421ed04b9fa137145eaf7b1702

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 36 h
  2. 2
    其他The solvent was removed in vacuo
  3. 3
    其他the residue was purified by column chromatography on silica gel (ethyl acetate in petroleum ether, 1% v/v)

实验过程

A mixture of 5-bromo-2-methylpyrimidine (100 mg, 0.58 mmol), NBS (103 mg, 0.58 mmol), dibenzoyl peroxide (10 mg, 0.04 mmol) in tetrachloromethane (10 mL) was refluxed for 36 h. The solvent was removed in vacuo and the residue was purified by column chromatography on silica gel (ethyl acetate in petroleum ether, 1% v/v) to give 5-Bromo-2-(bromomethyl)pyrimidine (70 mg, 48%) as a white solid. 1HNMR (400 MHz, CDCl3) δ 4.49 (s, 2H), 8.72 (s, 2H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08367663B2uspto-grants-2013_02