HRID57559

反应详情

EQUATION

反应方程式

HRID 57559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a mixture of 1-fluoro-4-nitrobenzene (5.64 g, 40.0 mmol) and potassium carbonate (11.1 g, 80.0 mmol) in DMSO (30 mL) was added 2-methylmorpholine (4.05 g, 40.0 mmol), then the mixture was heated at 100° C. for 4 hours. This solution was poured on to water (300 mL) and extracted with EA (3×100 mL). The combined organic phase was washed with brine and dried. Filtered and Pd/C (1.0 g) was added to the filtrate, charged with H2, and stirred at room temperature overnight. The catalyst was filtered and the filtrate was concentrated to give product as a light red solid. MS (m/z): 193 (M+H)+.

WORKUP

后处理

  1. extractionextracted with EA (3×100 mL)
  2. washThe combined organic phase was washed with brine
  3. customdried
  4. filtrationFiltered
  5. additionPd/C (1.0 g) was added to the filtrate
  6. additioncharged with H2
  7. filtrationThe catalyst was filtered
  8. concentrationthe filtrate was concentrated
  9. customto give product as a light red solid