HRID905574

反应详情

EQUATION

反应方程式

HRID 905574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

2,4,6-Trifluoronitrobenzene (4.95 g) and potassium carbonate (4.63 g) were mixed in dry dimethyl sulfoxide (40 mL) and cooled to 10° C. under argon. Morpholine (2.56 mL) was added and the reaction mixture was allowed to warm to 25° C. and stirred under argon for 16 hours. The reaction mixture was concentrated in vacuo Brine (50 mL) was added and the product was extracted with ethyl acetate (3×50 mL). The combined organic phases were dried over magnesium sulfate and concentrated in vacuo). The crude material was purified by flash chromatography to furnish 2.49 g (37% yield) of the title compound as a yellow solid. 1H NMR (500 MHz, DMSO-d6): 3.43 (t, 4H), 3.69 (t, 4H), 6.87 (d, 2H).

WORKUP

后处理

  1. temperatureto warm to 25° C.
  2. concentrationThe reaction mixture was concentrated in vacuo Brine (50 mL)
  3. additionwas added
  4. extractionthe product was extracted with ethyl acetate (3×50 mL)
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. concentrationconcentrated in vacuo)
  7. customThe crude material was purified by flash chromatography