反应详情

温度

45 °C

A solution of the product (140 mg, 0.385 mmol) from Step B in 1.5 mL of dry dichloromethane was treated with 1-chloroethyl chloroformate (0.050 mL, 0.46 mmol). The reaction mixture was warmed to 45° C. After 20 h, the solution was cooled to room temperature and concentrated under a stream of nitrogen. The resultant residue was dissolved in 3 mL of methanol and the solution was warmed at 40° C. for 2.5 h. The resultant solution was cooled and concentrated under a stream of nitrogen, and the residue was triturated with 4 mL of ethyl acetate. The solid precipitate was collected and dried in vacuo to afford the title compound as a white crystalline solid. LC/MS 275.0 (M+1).

1. temperaturethe solution was cooled to room temperature
2. concentrationconcentrated under a stream of nitrogen
3. dissolutionThe resultant residue was dissolved in 3 mL of methanol
4. temperaturethe solution was warmed at 40° C. for 2.5 h
5. temperatureThe resultant solution was cooled
6. concentrationconcentrated under a stream of nitrogen
7. customthe residue was triturated with 4 mL of ethyl acetate
8. customThe solid precipitate was collected
9. customdried in vacuo