反应详情

A 100 mg sample of 13-fluoro-1,4,7,10-tetraaza-13-phosphatetracyclo[5.5.1.04,13.010,13 ]tridecane was dissolved in 0.5 ml of 1N sodium hydroxide by heating to near boiling. This mixture was cooled, filtered and evaporated. The white residue was then sublimed at 150°-180° and 0.1 mm pressure to give 90 mg of 13-oxo-1,4,7,10-tetraaza-13-phosphatricyclo[5.5.1.04,13 ]tridecane and leaving 10- 20 mg of residue. The sublimate was kept under dry nitrogen and melted at 215°-217° to a clear colorless melt. On exposure to moist air this solid picked up water of hydration without softening. The hydrated sample softened at 90° and slowly lost water up to 160° where the sample frothed and then darkened and totally melted in the range of 200°-210°. The anhydrous sample was used for nmr and mass spectra.

1. temperatureby heating to near boiling
2. temperatureThis mixture was cooled
3. filtrationfiltered
4. customevaporated
5. customwas then sublimed at 150°-180°