HRID483286

反应详情

EQUATION

反应方程式

HRID 483286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4'-Trifluoromethyl-2-biphenylcarbaldehyde (1.08 g, 4.32 mmol) in tert-butanol (15 mL) at 80° C. was added a solution of potassium permanganate (0.89 g, 5.62 mmol) in water (25 mL). After stirring at 80° C. for two hours, the mixture was cooled, a solution of 3N sodium hydroxide was added (2 mL) and the manganese dioxide was filtered off. The filtrate was diluted with water (15 mL) and acidified with 6N hydrochloric acid to precipitate the title compound (1.05 g, 91.2%). Dissolution in 0.3N sodium hydroxide (15 mL), followed by charcoal treatment, filtrating, and precipitation with 6N hydrochloric acid gave the purified 4-Trifluoromethyl-2-biphenylcarboxylic acid compound (0.85 g, 85%). 'H NMR (CDCl3): 7.5 (m, 7, ArH), 8.0 (m, 1,3-H), 9.5 (broad s, 1, CO2H).

WORKUP

后处理

  1. temperaturethe mixture was cooled
  2. filtrationthe manganese dioxide was filtered off
  3. additionThe filtrate was diluted with water (15 mL)
  4. customto precipitate the title compound (1.05 g, 91.2%)
  5. dissolutionDissolution in 0.3N sodium hydroxide (15 mL)
  6. filtrationfiltrating
  7. customprecipitation with 6N hydrochloric acid