反应详情

To a solution of methyl [4-(2-{(1S,2R)-2-[1-(5-ethylpyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethoxy)-2-fluorophenyl]acetate (0.300 g, 0,679 mmol) in 6 ml anhydrous tetrahydrofuran was added by 2 ml methanol and 2 ml water. Lithium hydroxide (81.0 mg, 3.40 mmol) was added, and the mixture stirred at RT overnight. 1 M hydrochloric acid was added and the pH adjusted to 4. The volatiles were removed under reduced pressure, and the aqueous phase extracted with dichloromethane (3×20 ml). The organics were combined, dried over magnesium sulphate, filtered, and the filtrate concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (50 g silica gel) using a gradient eluent of 0-70% ethyl acetate in hexanes (700 ml) to afford the title compound. LC/MS (m/z) 428.2 (M+H)+.

1. customThe volatiles were removed under reduced pressure
2. extractionthe aqueous phase extracted with dichloromethane (3×20 ml)
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel (50 g silica gel)