反应详情

A mixture of 430D (1.24 g, 3.0 mmol), Et3N (1.67 ml, 12.0 mmol) and DPPA (1.29 ml, 6.0 mmol) in 1,4-dioxane (20 ml) was stirred at rt for 16 h under argon. Benzyl alcohol (1.86 ml, 18.0 mmol) was added. The resulting mixture was heated to 80° C. for 2.5 h, cooled to rt. Removal of the solvent in vacuo gave a brown oil. Treated with EtOAc (100 ml), the mixture was washed with H2O (3×30 ml) and brine (20 ml), dried with Na2SO4. Removal of the solvent followed by flash chromatography of the residue on silica gel (CH2Cl2 first, then 20% EtOAc-hexanes) gave 430E (1.17 g, 75%) as a light yellow solid. It has a retention time of 6.96 min (standard LC1 method, 8 min run). MS Found: (M+H)+=520.2

1. temperatureThe resulting mixture was heated to 80° C. for 2.5 h
2. temperaturecooled to rt
3. customRemoval of the solvent in vacuo
4. customgave a brown oil
5. washthe mixture was washed with H2O (3×30 ml) and brine (20 ml)
6. dry with materialdried with Na2SO4
7. customRemoval of the solvent