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温度

0 °C

Compound 6, prepared in Example 1 (v) above (6.122 g, 13.4 mmoL), was treated with TFA (13 mL) in dichloromethane (80 mL) at room temperature. After 2 h, the reaction mixture was washed with 2M sodium hydroxide (25 mL) and the organic layer was separated. The organic layer was dried (MgSO), filtered and concentrated. The residue was dissolved in dichloromethane (120 mL), cooled to 0° C. and benzyl bromide (1.8 mL, 15.1 mmol) and triethylamine (5.7 mL, 41.0 mmol) were added. The reaction was gradually warmed to room temperature and after 20 hours the reaction was washed with water (1×100 mL). The organic layer was dried (MgSO4), filtered and concentrated. Purification by flash chromatography, eluting 50 to 60% ethyl acetate in hexanes gave 3.80 g of product (64% yield).

1. washthe reaction mixture was washed with 2M sodium hydroxide (25 mL)
2. customthe organic layer was separated
3. dry with materialThe organic layer was dried (MgSO)
4. filtrationfiltered
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in dichloromethane (120 mL)
7. temperatureThe reaction was gradually warmed to room temperature and after 20 hours the reaction
8. washwas washed with water (1×100 mL)
9. dry with materialThe organic layer was dried (MgSO4)
10. filtrationfiltered
11. concentrationconcentrated
12. customPurification by flash chromatography
13. washeluting 50 to 60% ethyl acetate in hexanes