HRID1766440

反应详情

EQUATION

反应方程式

HRID 1766440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Methyl-2(1H)-pyridinone (50 g, 0.46 mol) was suspended in dichloromethane (500 mL). N-bromosuccinimide (82 g, 0.46 mol) was added in portions with cooling. Addition was finished after 15 min; the mixture was stirred for 1 h at room temperature and afterwards partitioned between dichloromethane and water. Organic phases were pooled, dried with Na2SO4 and the solvent was evaporated. The residue was purified by crystallization from ethyl acetate to yield 55 g of the title compound as a light yellow solid, mp 156–161° C.

WORKUP

后处理

  1. temperaturewith cooling
  2. additionAddition
  3. customafterwards partitioned between dichloromethane and water
  4. dry with materialdried with Na2SO4
  5. customthe solvent was evaporated
  6. customThe residue was purified by crystallization from ethyl acetate