Hydrazine hydrate (1:1) → HCID 21317713, compound
Reaction equation
[Cl:1][C:2]1[S:18][C:5]2[NH:6][C:7](=S)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1.O.[NH2:20][NH2:21]>CO>[Cl:1][C:2]1[S:18][C:5]2[N:6]=[C:7]([NH:20][NH2:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
1.1 g (0.00376 mol) of 7-chloro-1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepine-2-thione are dissolved in 400 ml of absolute methanol with warming and 1 ml of 100% hydrazine hydrate is added. The solution is concentrated to 50 ml and left to crystallize in a refrigerator. After filtration under vacuum and drying, there is obtained 7-chloro-2-hydrazino-5-phenyl-3H-thieno[2,3-e]-1,4-diazepine as colorless crystals, melting at 204°-207° C. (decomposition from 185° C.).
Workup
- temperaturewith warming
- concentrationThe solution is concentrated to 50 ml
- waitleft
- customto crystallize in a refrigerator
- filtrationAfter filtration under vacuum
- customdrying
Sources & evidence
- ORD record
- ord-3d1314e402574954b853bbc6504c0aed
- Source dataset
- uspto-grants-1979_05
- Patent number
- US04155913
Reaction notes
Loading…