HRID2401215

反应详情

EQUATION

反应方程式

HRID 2401215 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-5-methyl-6-[(methyloxy)methyl]pyrimidine (Intermediate 49, 2.14 g, 12.40 mmol) was dissolved in DCM (105 ml), cooled in an ice bath and treated with 1M boron tribromide in DCM (13.64 ml, 13.64 mmol). The resulting mixture was stirred for 1 hour, allowed to warm to room temperature and stirred for 1 hour. The reaction was quenched by adding water and diluted with DCM. The DCM layer was separated, dried under magnesium sulfate and evaporated under reduced pressure to give the title compound as a yellow solid (1.70 g) m/z (ES+) 159 (M+1), title compound is 49% pure by LCMS. Also contains (6-bromo-5-methyl-4-pyrimidinyl)methanol, m/z (ES+) 203, 205 (M+1) (49% by LCMS)

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. stirringstirred for 1 hour
  3. customThe reaction was quenched
  4. additionby adding water
  5. additiondiluted with DCM
  6. customThe DCM layer was separated
  7. customdried under magnesium sulfate
  8. customevaporated under reduced pressure