Sodium Hydroxide → HCID 15371246, compound

HRID 1288214Notes

Reaction equation

HRID 1288214 reaction equation
F[P:2]123[N:12]4[CH2:13][CH2:14][N:3]1[CH2:4][CH2:5][N:6]2[CH2:7][CH2:8][N:9]3[CH2:10][CH2:11]4.[OH-:15].[Na+]>>[O:15]=[P:2]12[N:9]3[CH2:10][CH2:11][NH:12][CH2:13][CH2:14][N:3]1[CH2:4][CH2:5][N:6]2[CH2:7][CH2:8]3

Participants

3

Reactant 2

HCID 14798Sodium HydroxideHCID 12872714HCID 12872714, compound

Product 1

HCID 15371246HCID 15371246, compound

Procedure

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.

Workup

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

Sources & evidence

ORD record
ord-93a267dce6624248af974ec74e6eba6b
Source dataset
uspto-grants-1976_10
Patent number
US03987128

Reaction notes

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