HRID1485685

反应详情

EQUATION

反应方程式

HRID 1485685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A 200-mL round bottomed flask equipped with a magnetic stir bar was charged with 1-fluoro-2-nitrobenzene (8.25 g, 58.5 mmol), DMSO (29 mL), potassium carbonate (8.89 g, 64.3 mmol), and (S)-2-aminopropane-1-ol (4.83 g, 64.3 mmol). The mixture was heated to 60° C. for 6 h and then cooled to room temperature. The reaction mixture was diluted with water (60 mL). The mixture was stirred for several minutes, then extracted with ethyl acetate (ca. 200-250 mL). The ethyl acetate extract was washed thrice with 5 wt % aqueous sodium chloride (3×50 mL) and concentrated under reduced pressure to afford crude (S)-2-(2-nitrophenylamino)propane-1-ol (12.0 g, 105%) as a bright orange syrup. MS (ESI, pos. ion) m/z 197 [M+1]+.

WORKUP

后处理

  1. customA 200-mL round bottomed flask equipped with a magnetic stir bar
  2. temperaturecooled to room temperature
  3. extractionextracted with ethyl acetate (ca. 200-250 mL)
  4. extractionThe ethyl acetate extract
  5. washwas washed thrice with 5 wt % aqueous sodium chloride (3×50 mL)
  6. concentrationconcentrated under reduced pressure