反应详情

0.71 ml of trimethylsilyl bromide is added at 0° to a solution of 123 mg of 9 in 3 ml of dichloromethane. After stirring at 0° for 4 hours, 20 ml of water are added. After 30 minutes, the dichloromethane phase is separated off and washed three times with 15 ml of water each time. The aqueous phases are extracted three times with 20 ml of dichloromethane each time and concentrated by evaporation in vacuo. The residue is dissolved in 10 ml of 5N hydrochloric acid and is then stirred for 48 hours, diluted with 20 ml of water and extracted three times with 20 ml of dichloromethane each time. The aqueous phase is concentrated by evaporation in vacuo, and the residue is dried under a high vacuum and dissolved in 3 ml of etharol, and then approximately 1 ml of propylene oxide is added dropwise thereto. The suspension is filtered. Washing of the filtration residue with ethanol and drying under a high vacuum at roomtemperature yields 62 mg of 10, m.p. 165° C. (decomposition).

1. waitAfter 30 minutes
2. customthe dichloromethane phase is separated off
3. washwashed three times with 15 ml of water each time
4. extractionThe aqueous phases are extracted three times with 20 ml of dichloromethane each time
5. concentrationconcentrated by evaporation in vacuo
6. dissolutionThe residue is dissolved in 10 ml of 5N hydrochloric acid
7. stirringis then stirred for 48 hours
8. additiondiluted with 20 ml of water
9. extractionextracted three times with 20 ml of dichloromethane each time
10. concentrationThe aqueous phase is concentrated by evaporation in vacuo
11. customthe residue is dried under a high vacuum
12. dissolutiondissolved in 3 ml of etharol
13. additionapproximately 1 ml of propylene oxide is added dropwise
14. filtrationThe suspension is filtered
15. washWashing of the filtration residue with ethanol
16. customdrying under a high vacuum at roomtemperature