反应详情

Potassium hydroxide (2.976 g) in water (30 mL) was added to a suspension of 2-chloro-3-(cyanomethyl)benzoic acid (example 80, step a) (4.12 g) in ethanol (30 mL) and the resulting solution was heated at reflux for 2 hours, then allowed to cool overnight. The mixture was concentrated in vacuo to remove the ethanol and then diluted with water and washed twice with ethyl acetate. The organic phases were discarded, whilst the aqueous phase was acidified to pH 1 with concentrated hydrochloric acid and extracted three times with ethyl acetate. The combined extracts were dried over anhydrous magnesium sulphate and concentrated in vacuo to afford the crude subtitled compound as a yellow solid. Yield 4.11 g. Used directly.

1. temperaturethe resulting solution was heated
2. temperatureat reflux for 2 hours
3. temperatureto cool overnight
4. concentrationThe mixture was concentrated in vacuo
5. customto remove the ethanol
6. additiondiluted with water
7. washwashed twice with ethyl acetate
8. extractionextracted three times with ethyl acetate
9. dry with materialThe combined extracts were dried over anhydrous magnesium sulphate
10. concentrationconcentrated in vacuo