反应详情

A solution of D9 (0.39 g, 1.4 mmole) in DCM (30 ml) was treated with iPr2EtN (0.26 g, 2 mmole) followed by 1-chloroethyl chloroformate (0.29 g, 2 mmole) and stirred at room temperature for 3 h, then concentrated under vacuum and the residue treated with MeOH (30 ml) and heated under reflux for 1 h. The mixture was allowed to cool and the solid filtered off, washed with Et2O and dried. This was treated with 10% Na2CO3 solution, extracted with DCM and the extract dried and concentrated under vacuum to afford the title compound as a colourless oil (0.33 g, 88%).

1. concentrationconcentrated under vacuum
2. additionthe residue treated with MeOH (30 ml)
3. temperatureheated
4. temperatureunder reflux for 1 h
5. temperatureto cool
6. filtrationthe solid filtered off
7. washwashed with Et2O
8. customdried
9. additionThis was treated with 10% Na2CO3 solution
10. extractionextracted with DCM
11. customthe extract dried
12. concentrationconcentrated under vacuum