反应详情

Lithium hydroxide (13.3 mg, 0.554 mmol) in water (1.5 ml) was added into 70335 methyl 2-[(4-{2-[(2,4-difluorobenzyl)(heptyl)amino]-2-oxoethyl}phenoxy)methyl]benzoate (145 mg, 0.277 mmol) dissolved in THF (3 ml). The mixture was then in microwave oven (Smith Synthesizer) at 150° C. for 7 minutes and then evaporated to remove THF. The residue was acidified with 1% hydrochloric acid, pH˜4 and then extracted with ethyl acetate (×2). The organic portions were combined, washed with brine, dried with magnesium sulphate and then evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 2 g/6 ml) using DCM then MeOH/DCM (0.5:99.5, then 1:99) as eluant gave 94 mg desired product, yield 67%.

1. customevaporated
2. customto remove THF
3. extractionextracted with ethyl acetate (×2)
4. washwashed with brine
5. dry with materialdried with magnesium sulphate
6. customevaporated