反应详情

Intermediate 17 (0.25 g, 0.86 mmol), EDC (0.23 g, 1.2 mmol) and HOBT (0.139 g, 1.03 mmol) were suspended in DMF (5 ml) and the suspension was stirred at room temperature. After 25 min, (2R)-2-Amino-2-phenylethanol (0.13 g, 0.95 mmol, commercially available from Aldrich) was added, and the mixture was stirred at room temperature for 20 hours. Solvents were removed in vacuo and the residue was dissolved in DCM (50 ml) and washed successively with water (25 ml) and 5% sodium hydrogen carbonate solution (25 ml). The organic layer was dried over anhydrous sodium sulphate and concentrated in vacuo. The residue was dissolved in dichloromethane (5 ml) and applied to a SPE cartridge (silica, 10 g), which was eluted with a gradient of ethyl acetate—petroleum ether (1:2, 1:1 and 1:0). Fractions containing the desired material were combined and concentrated in vacuo to afford Intermediate 42 as a white foam (0.318 g). LCMS showed MH+=410; TRET=2.55 min.

1. stirringthe mixture was stirred at room temperature for 20 hours
2. customSolvents were removed in vacuo
3. dissolutionthe residue was dissolved in DCM (50 ml)
4. washwashed successively with water (25 ml) and 5% sodium hydrogen carbonate solution (25 ml)
5. dry with materialThe organic layer was dried over anhydrous sodium sulphate
6. concentrationconcentrated in vacuo
7. dissolutionThe residue was dissolved in dichloromethane (5 ml)
8. washwas eluted with a gradient of ethyl acetate—petroleum ether (1:2, 1:1 and 1:0)
9. additionFractions containing the desired material
10. concentrationconcentrated in vacuo