HRID2186476

反应详情

EQUATION

反应方程式

HRID 2186476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of D-Proline anilide (1.15 g, 6.0 mmol) in 20 mL of THF at 0° C. was added a 1 M solution of lithium aluminum hydride (14 mL, 14 mmol) in THF. The resulting solution was stirred at 0° C. for 11 hours. The reaction was carefully quenched with a saturated solution of Na2SO4 and extracted with EtOAc. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give the title compound as an oil. The oil was purified by silica gel chromatography with 3% CH3OH/CH2Cl2 and 1% triethyl amine to give the title compound as a yellow oil (0.029 g, 63%). ES (+) MS m/e=177 (M+H)

WORKUP

后处理

  1. customThe reaction was carefully quenched with a saturated solution of Na2SO4
  2. extractionextracted with EtOAc
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure