反应详情

To a stirred solution of 36-2 (0.15 g, 0.52 mmol) in dichloromethane (2 mL) was added triethylamine (0.15 mL, 1.08 mmol) and methanesulfonyl chloride (0.05 mL, 0.62 mmol). The resulting mixture was stirred at room temperature for 10 minutes and concentrated. The residue was dissolved in DMF (2 mL). To this solution was added sodium azide (0.20 g, 3.08 mmol) and the mixture was heated to 90° C. for 3 days. The reaction was allowed to cool and partitioned between ethyl acetate and water. The organic phase was concentrated to give 36-3. (0.13 g, 83%). LRMS (ES) (M+H)+: observed=317.1, calculated=317.4.

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in DMF (2 mL)
3. temperaturethe mixture was heated to 90° C. for 3 days
4. temperatureto cool
5. custompartitioned between ethyl acetate and water
6. concentrationThe organic phase was concentrated
7. customto give 36-3