Cyanogen Bromide → HCID 15107886, compound
Reaction equation
[Cl:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]([NH:12][NH2:13])=[N:4][N:3]=1.C([O-])(=O)C.[Na+].[N:19]#[C:20]Br>CO>[NH2:19][C:20]1[N:4]2[N:3]=[C:2]([Cl:1])[C:11]3[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[C:5]2=[N:12][N:13]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A 46.88 gm (0.236 mole) quantity of 1-chloro-4-hydrazino5,6,7,8-tetrahydrophthalazine was added to 450 ml of methanol. A 40.8 gm quantity of sodium acetate and 25.0 gm of cyanogen bromide was added and the mixture was stirred on a warm plate for 30 minutes. Yellow crystals appeared immediately. The mixture was allowed to sit for 3 days. The resulting solid was filtered, washed with ether, and dried, yielding 44.85 gm of 3-amino-6-chloro-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine; mp 224-225° C. (ethanol).
Workup
- waitto sit for 3 days
- filtrationThe resulting solid was filtered
- washwashed with ether
- customdried
Sources & evidence
- ORD record
- ord-97d0a16047ce42a3989ca1f536f1bb0a
- Source dataset
- uspto-grants-1991_04
- Patent number
- US05011835
Reaction notes
Loading…