HRID525589

反应详情

EQUATION

反应方程式

HRID 525589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a stirred solution of (4S,5R)-5-[4-(6-Dimethylcarbamoyl-pyridin-3-yl)-phenyl]-4-fluoromethyl-2,2-dimethyl-oxazolidine-3-carboxylic acid tert-butyl ester (260 mg, 0.569 mmol) in dry tetrahydrofuran (6.5 mL) is added 2M toluene solution BH3.DMS (130 mg, 1.708 mmol) at 0° C. Reaction heated to 65° C. for 16 hours. Methanol is added to reaction mixture and heated at 65° C. for 2 hours. Volatiles are removed under reduced pressure to obtain crude material purified by column chromatography eluting in 5% methanol in CH2Cl2 to afford the title compound (50 mg): LC-MS (m/z): [M+H]=444.

WORKUP

后处理

  1. customat 0° C
  2. customReaction
  3. temperatureheated at 65° C. for 2 hours
  4. customVolatiles are removed under reduced pressure
  5. customto obtain crude material
  6. custompurified by column chromatography
  7. washeluting in 5% methanol in CH2Cl2