反应详情

Methyl 2-{[3-(2-oxo-2-{[4-(trifluoromethyl)benzyl]amino}ethyl)phenoxy]methyl}-benzoate (82 mg, 0.18 mmol) in THF (2 ml) was cooled in an ice-bath. Lithium hydroxide (8.6 mg, 0.36 mmol) in water (1 ml) was dropped in. The cooling-bath was then removed and the mixture was stirred for 7 days and then evaporated in vacuum to remove THF. The residue was acidified with 1% hydrochloric acid, pH˜3, and extracted with ethyl acetate. The organic phase was dried (magnesium sulphate) and evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 2 g/6 ml) using DCM and MeOH/DCM (1:99, then 2:98) as eluant gave 20 mg the desired product, yield 22.5% (two steps).

1. customThe cooling-bath was then removed
2. customevaporated in vacuum
3. customto remove THF
4. extractionextracted with ethyl acetate
5. dry with materialThe organic phase was dried (magnesium sulphate)
6. customevaporated