HRID2401215
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
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
- temperaturecooled in an ice bath
- stirringstirred for 1 hour
- customThe reaction was quenched
- additionby adding water
- additiondiluted with DCM
- customThe DCM layer was separated
- customdried under magnesium sulfate
- customevaporated under reduced pressure