反应详情

温度

40 °C

Add 1M lithium aluminum hydride in tetrahydrofuran (121 mL, 121 mmol) to anhydrous tetrahydrofuran (100 mL) under argon gas. Warm the reaction mixture to 40° C. and add in small portions 4-cyano-3-fluorobenzoic acid (5.0 g, 30.28 mmol) over a 1 hr period. Stir the reaction mixture at 40° C. for 4 hrs and then at room temperature overnight. Cool the reaction mixture to 0° C. and quench by the sequential addition of water (5 mL), 15% sodium hydroxide solution (17 mL), and water (5 mL). Allow the mixture to warm-up to room temperature and stir for 1 hr. Filter the precipitate through diatomaceous earth and concentrate the filtrate to provide the title compound (4.4 g, 28.4 mmol).

1. customat room temperature
2. customovernight
3. temperatureCool the reaction mixture to 0° C.
4. customquench by the sequential addition of water (5 mL), 15% sodium hydroxide solution (17 mL), and water (5 mL)
5. temperatureAllow the mixture to warm-up to room temperature
6. stirringstir for 1 hr
7. filtrationFilter the precipitate through diatomaceous earth
8. concentrationconcentrate the filtrate