HRID420750

反应详情

EQUATION

反应方程式

HRID 420750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was heated at 40° C. for 4 h
  2. filtrationThe suspension was filtered over nylon membrane 0.45 μm and it
  3. washwas rinsed with DCM
  4. customThe filtrate was evaporated under vacuum