Acetic Anhydride → HCID 178474260, compound
Reaction equation
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:4]=[C:5]([N:9]([C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][C:14]=2[C:20]2[NH:24][N:23]=[N:22][N:21]=2)[C:10]([NH2:12])=[O:11])[CH:6]=[CH:7][CH:8]=1.[C:27](OC(=O)C)(=[O:29])[CH3:28]>C([O-])(=O)C.[Na+]>[F:26][C:2]([F:1])([F:25])[C:3]1[CH:4]=[C:5]([N:9]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][C:27](=[O:29])[CH3:28])=[CH:15][C:14]=2[C:20]2[NH:24][N:23]=[N:22][N:21]=2)[C:10]([NH2:12])=[O:11])[CH:6]=[CH:7][CH:8]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
To a solution of 3-trifluoromethylphenyl-4-amino-2-(5-tetrazolyl)phenyl urea (0.22 g, 0.6 mmol) in 17% aqueous sodium acetate (5 mL), cooled on an ice bath, was added acetic anhydride (1 mL). The reaction was stirred at 0° C. for another hour. The precipitate was filtered off and re-crystallised from 96% ethanol to give 0.12 g of the desired material. M.p. 280-282° C.
Workup
- filtrationThe precipitate was filtered off
- customre-crystallised from 96% ethanol
Sources & evidence
- ORD record
- ord-1ecb3a8102704e4aaa5e602f91ffed1e
- Source dataset
- uspto-grants-2004_02
- Patent number
- US06696475B2
Reaction notes
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