反应详情

To a mixture of 1-methylethyl 4-[(1-methylethyl)oxy]-3-(trifluoromethyl)benzoate (D70) (704 mg, 2.43 mmol) in ethanol (110 mL) was added aqueous sodium hydroxide (2M, 12.2 mL, 24.3 mmol) and the reaction heated to reflux for 1 h. The mixture was concentrated in vacuo and the residue partitioned between ethyl acetate (100 mL) and water (100 mL) and acidified with aqueous hydrochloric acid (2M, 13 mL). The aqueous layer was extracted further with ethyl acetate (100 mL) and the combined organic layers dried and concentrated in vacuo to give the title compound as a yellow solid (563 mg). δH (methanol-d4, 400 MHz): 8.21-8.17 (2H, m), 7.26 (1H, d), 4.84 (1H, septet), 1.38 (6H, d). MS (ES): C11H11F3O3 requires 248; found 247 (M−H+).

1. temperaturethe reaction heated
2. temperatureto reflux for 1 h
3. concentrationThe mixture was concentrated in vacuo
4. customthe residue partitioned between ethyl acetate (100 mL) and water (100 mL)
5. extractionThe aqueous layer was extracted further with ethyl acetate (100 mL)
6. customthe combined organic layers dried
7. concentrationconcentrated in vacuo