反应详情

Methyl 2-[(3-{2-[benzyl(hexyl)amino]-2-oxoethyl}phenoxy)methyl]benzoate (59 mg, 0.125 mmol) in THF (1 ml) was cooled in an ice-bath. Lithium hydroxide (6 mg, 0.249 mmol) in water (1 ml) was dropped in. The cooling-bath was then removed and the mixture was stirred for 13 days and then evaporated in vacuum to remove THF. The residue was acidified with 1% hydrochloric acid, pH˜4, and extracted with ethyl acetate. The organic phase was dried (magnesium sulphate) and evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 1 g/6 ml) using DCM and MeOH/DCM (0.5:99.5, then 1:99) as eluant gave 7 mg the desired product, yield 8% (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