反应详情

To 3 (835 mg, 6 mmol) in suspension in tetrahydrofuran (7 mL) was successively added, under an argon atmosphere, 4-dimethylaminopyridine (18.3 mg; 0.15 mmol), triethylamine (0.84 mL; 6 mmol) and BOC2O (2.62 g; 12 mmol). The reaction mixture was stirred at room temperature for 3 days. The solvent was removed under vacuum. The residue was diluted with diethyl ether (20 mL) and washed with water (2×10 mL). The phases were separated, and the organic phase was dried over MgSO4 and concentrated. The crude oil was purified over silica gel chromatography (ether/heptane 1:1) to give 4 (986 mg; 4.1 mmol; 70%) as a white solid.

1. customThe solvent was removed under vacuum
2. additionThe residue was diluted with diethyl ether (20 mL)
3. washwashed with water (2×10 mL)
4. customThe phases were separated
5. dry with materialthe organic phase was dried over MgSO4
6. concentrationconcentrated
7. customThe crude oil was purified over silica gel chromatography (ether/heptane 1:1)
8. customto give 4 (986 mg; 4.1 mmol; 70%) as a white solid