反应详情

4-Hydroxy-benzoic acid tert-butyl ester (0.65 g, 3.08 mmol) was dissolved in acetonitrile (7.5 ml) and added to 2-(10-Bromodecanoylamino) pentanedioic acid 5-benzyl ester 1-tert-butyl ester (1.62 g, 3.08 mmol). Acetonitrile (90 ml) and K2CO3 (0.64 g, 4.62 mmol) was added and the mixture was refluxed for 16 h under a flow of N2. The solvent was removed under vacuum. AcOEt (100 ml) was added and the solution was washed with water (2×50 ml) using sat. NaCl and methanol to aid phase separation, dried over MgSO4, and concentrated to yield a light brown oil (2.18 g). The oil was purified by flash chromatography (silica, 95:5 DCM/AcOEt) to yield an oil (160 mg, 8%).

1. customThe solvent was removed under vacuum
2. additionAcOEt (100 ml) was added
3. washthe solution was washed with water (2×50 ml)
4. customphase separation
5. dry with materialdried over MgSO4
6. concentrationconcentrated