Water → HCID 21286378, compound
Reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([N:20]2[C:25](=[O:26])[NH:24][C:23](=[O:27])[CH2:22][NH:21]2)[CH:5]=[C:6]([Cl:19])[C:7]=1[O:8][C:9]1[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=1.S(=O)(=O)(O)O.O.[C:34](OC(=O)C)(=[O:36])[CH3:35]>>[C:34]([N:21]1[CH2:22][C:23](=[O:27])[NH:24][C:25](=[O:26])[N:20]1[C:4]1[CH:5]=[C:6]([Cl:19])[C:7]([O:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][CH:14]=2)=[C:2]([Cl:1])[CH:3]=1)(=[O:36])[CH3:35]Participants
5
Procedure
2 g of 2-[3,5-dichloro-4-(4-methylsulfonylphenoxy)phenyl]hexahydro-1,2,4-triazine-3,5-dione were suspended in 10 ml of acetic anhydride. 1 ml of concentrated sulfuric acid was added dropwise, during which there was a slight increase in the temperature of the suspension and the starting material slowly dissolved. The mixture was then stirred at room temperature for 2 to 3 hours, and was subsequently stirred with water. The product was filtered off with suction, washed with water and dried, and recrystallized from a little glacial acetic acid, melting point 267° C.
Workup
- temperaturea slight increase in the temperature of the suspension
- dissolutionthe starting material slowly dissolved
- filtrationThe product was filtered off with suction
- washwashed with water
- customdried
- customrecrystallized from a little glacial acetic acid, melting point 267° C.
Sources & evidence
- ORD record
- ord-0b1688980ddd43378d5fa808086afb80
- Source dataset
- uspto-grants-1988_11
- Patent number
- US04782056
Reaction notes
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