HRID1059666

反应详情

EQUATION

反应方程式

HRID 1059666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

To a stirred solution of 3-hydroxyaniline (6.55 g) and 4-fluorobenzotrifluoride (9.85 g) in DMSO (50 mL) was added in one portion potassium tert-butoxide (7.86 g). The resulting dark solution was heated for 4 hours at 95° C., cooled to room temperature, then poured into water (600 mL). The mixture was extracted with ether (3×125 mL). The organic phase was washed with 2N sodium hydroxide (2×75 mL) and water (100 mL), dried (MgSO4) and the solvent evaporated to give a dark oil. This oil was distilled to give the title aniline as a colorless oil (8.7 g), b.p. 110-112° C. at 0.15 mm.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. extractionThe mixture was extracted with ether (3×125 mL)
  3. washThe organic phase was washed with 2N sodium hydroxide (2×75 mL) and water (100 mL)
  4. dry with materialdried (MgSO4)
  5. customthe solvent evaporated
  6. customto give a dark oil
  7. distillationThis oil was distilled