反应详情

温度

80 °C

A mixture of 80B (650 mg, 1.53 mmol) and sodium azide (597 mg, 9,18 mmol) was heated at 80° C. for 2 days. The reaction was diluted with EtOAc (200 mL), washed with brine:water (1:1, 4×15 mL), dried (MgSO4), filtered and concentrated to give the crude product. Purification by chromatography (40 g ISCO silica gel cartridge, 0-20% EtOAc/hexane) provided 80C as a colorless oil (410 mg). MS (ES) m/z 271 [M−Boc+H]+.

1. washwashed with brine:water (1:1, 4×15 mL)
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto give the crude product
6. customPurification by chromatography (40 g ISCO silica gel cartridge, 0-20% EtOAc/hexane)