Hydrazine → HCID 131719149, compound
Reaction equation
[N+:1]([NH:4][C:5]1[C:9]([N+:10]([O-:12])=[O:11])=[N:8][O:7][N:6]=1)([O-:3])=[O:2].[NH2:13][NH2:14]>O>[NH:4]([C:5]1[C:9]([N+:10]([O-:12])=[O:11])=[N:8][O:7][N:6]=1)[N+:1]([O-:3])=[O:2].[NH3+:13][NH2:14]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Into a clean 250 ml 3 neck round bottom flask equipped with a nitrogen port, magnetic stirring bar, and thermocouple was placed 3-nitroamino-4-nitrofurazan ("ANF"; 4.44 grams 0.025M). Thirty-five mls of distilled water was then added and the flask set into an ice bath. Fuming hydrazine (95%; 0.942 g; 0.028M) was preweighed into a vial, then added over three minutes while not letting the reaction temperature exceed +8° C. The reaction mixture was kept cold for 10 minutes, then the ice bath was withdrawn and the reaction mixture was stirred 2.5 hrs. After transfer to a tarred one neck flask, the water was removed in vacuo at 40° C. to obtain crystals (94% yield). The crystals were dissolved in approximately 200 ml THF at 40° C. then the amount of solvent present was reduced and thereafter the solution was refrigerated at -20° C. for 16 hrs. The resulting yellow green crystals were collected and placed over high vacuum (68.5% theoretical yield). DSC: decomposition at 184° C. FTIR 3500-3000 (m), 1583 (s), 1467, 1422, 1395, 1348, 1296 (m). The density of the hydrate (X-ray analysis) was 1,704 g/ml.
Workup
- customthe flask set into an ice bath
- additionthen added over three minutes while not
- customexceed +8° C
- customthe ice bath was withdrawn
- customAfter transfer to a tarred one neck flask, the water was removed in vacuo at 40° C.
Sources & evidence
- ORD record
- ord-72fc6372bfbc414aa50bfa7971f7da89
- Source dataset
- uspto-grants-1995_10
- Patent number
- US05460669
Reaction notes
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