反应详情

To a solution of triphosgene (0.246 g, 0.804 mmol) in THF (5 mL) at 0° C. was added a mixture of 1-6 (0.78 g, 2.29 mmol), triethylamine (0.36 mL, 3.09 mmol) and THF (1 mL) over 10 minutes. After 30 minutes, the reaction was allowed to warm to ambient temperature and stir for 1 hour. The mixture was then purged with argon for 30 minutes, and to it was added a mixture of 3-6 (0.435 g, 2.52 mmol), triethylamine (0.36 mL, 3.09 mmol) and THF (5 mL). The mixture was then heated at 0° C. for 2 hours, allowed to cool to ambient temperature. 2M H2SO4 (2.5 mL) was then added, and the mixture stirred for 15 hours. The reaction was then quenched with a 10% w/v solution of K2CO3 (10 mL), diluted with ethyl acetate, washed with water and brine, dried over MgSO4, and concentrated to give 850 mg of 3-7 as a yellow oil, used crude in the next step.

1. customThe mixture was then purged with argon for 30 minutes
2. additionto it was added
3. temperatureThe mixture was then heated at 0° C. for 2 hours
4. temperatureto cool to ambient temperature
5. stirringthe mixture stirred for 15 hours
6. customThe reaction was then quenched with a 10% w/v solution of K2CO3 (10 mL)
7. additiondiluted with ethyl acetate
8. washwashed with water and brine
9. dry with materialdried over MgSO4
10. concentrationconcentrated