HRID420750
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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
To a solution of [5-bromo-6-(trifluoromethyl)-3-pyridinyl]methanol (155 mg, 0.605 mmol) in DCM (10 mL) was added CrO2 (Magtrieve) (1017 mg, 12.11 mmol). The suspension was heated at 40° C. in a pressure tube overnight. TLC showed starting material remaining, an excess of CrO2 (254 mg, 3.03 mmol) was added. The reaction mixture was heated at 40° C. for 4 h. The suspension was filtered over nylon membrane 0.45 μm and it was rinsed with DCM. The filtrate was evaporated under vacuum to afford 120 mg (78%) of title compound pure enough to be used in the next step.
WORKUP
后处理
- temperatureThe reaction mixture was heated at 40° C. for 4 h
- filtrationThe suspension was filtered over nylon membrane 0.45 μm and it
- washwas rinsed with DCM
- customThe filtrate was evaporated under vacuum