反应详情

温度

-40 °C

0.08 moles of triethylamine, 0.025 moles of POCl3 and 150 milliliters of dried tetrahydrofuran were combined in a 250 milliliter round bottom flask, under a nitrogen atmosphere to avoid moisture contamination, to form a first solution which was then cooled to -40° C. A second solution was then prepared containing 0.05 moles of 2,2-dimethylaziridine in 20 milliliters of THF and the second solution was added dropwise to the cooled first solution over a period of about 2 hours. The resulting slurry was then warmed over a period of about 1 hour to 0° C. then cooled again to -30° C. and then had added thereto, by dropwise addition, a solution containing 0.026 moles of 3-methoxypropyl amine in 20 milliliters of THF. The solution was then allowed to stand overnight with constant stirring at ambient temperature, the resulting slurry was filtered, the filtrate was concentrated by rotary evaporation, and thereafter vacuum distilled at 130° C./0.42 millimeters Hg to produce a 60% yield of 3-methoxypropylamino phosphoraziridine. NMR characterization indicated that the product was 95% pure.

1. customto form a first solution which
2. customA second solution was then prepared
3. additionthe second solution was added dropwise to the cooled first solution over a period of about 2 hours
4. temperatureThe resulting slurry was then warmed over a period of about 1 hour to 0° C.
5. temperaturethen cooled again to -30° C.
6. additionhad added
7. additionby dropwise addition
8. filtrationthe resulting slurry was filtered
9. concentrationthe filtrate was concentrated by rotary evaporation
10. distillationvacuum distilled at 130° C./0.42 millimeters Hg