HCID 11807266, compound → HCID 10923499, compound
Reaction equation
[N:1]([O-])=O.[Na+].[Cl:5][C:6]1[S:10][C:9]([S:11](=[O:14])(=[O:13])[NH2:12])=[C:8]([C:15]([NH:17][NH2:18])=[O:16])[CH:7]=1>O.Cl>[Cl:5][C:6]1[S:10][C:9]([S:11](=[O:13])(=[O:14])[NH2:12])=[C:8]([C:15]([N:17]=[N+:18]=[N-:1])=[O:16])[CH:7]=1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
A solution of sodium nitrite (3.0 g; 43.4 mmol) in 20 ml of water was added dropwise with stirring at 0° C. to a solution of 5-chloro-2-sulfamoylthiophene-3-carbohydrazide (10.0 g; 39.1 mmol) in 80 ml of 1M hydrochloric acid and the mixture was stirred for 15 min. The precipitate was isolated by filtration, washed with water and dried to give 9.93 g (96%) of the title compound; 1H-NMR (DMSO-d6): δ 7.55 (s, 1H), 7.97 (br. s, 2H, NH2).
Workup
- customThe precipitate was isolated by filtration
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-1d35f4b4f3a94869806d5e081ecd7e0e
- Source dataset
- uspto-grants-1999_03
- Patent number
- US05889002
Reaction notes
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