反应详情

To a solution of 3-chloro-5-trifluoromethoxybenzyl cyanide (6.3 g, 26.7 mmol; see step (ii) above) in 2-propanol (100 mL) was added water (200 mL) and potassium hydroxide (7.5 g, 133.5 mmol). The solution was refluxed for 18 h, cooled to room temperature, and the 2-propanol was removed in vacuo. The aqueous phase was washed with CH2Cl2 (2×) and the washings discarded. The basic aqueous phase was acidified with 2N HCl and extracted with CH2Cl2 (3×). The CH2Cl2 extracts were dried (Na2SO4), filtered and concentrated in vacuo to afford the sub-title compound (5.2 g, 76%) as an oil which was used in the next step without further purification.

1. temperatureThe solution was refluxed for 18 h
2. customthe 2-propanol was removed in vacuo
3. washThe aqueous phase was washed with CH2Cl2 (2×)
4. extractionextracted with CH2Cl2 (3×)
5. dry with materialThe CH2Cl2 extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo