Reaction equation
[OH-].[Na+].[N+:3]([C:6]1[CH:7]=[C:8]([S:27]([OH:30])(=[O:29])=[O:28])[C:9]([CH:12]=[CH:13][C:14]2[C:15]([S:23]([OH:26])(=[O:25])=[O:24])=[CH:16][C:17]([N+:20]([O-:22])=[O:21])=[CH:18][CH:19]=2)=[CH:10][CH:11]=1)([O-:5])=[O:4].[OH-].[K+:32].O=O.Cl>>[N+:20]([C:17]1[CH:16]=[C:15]([S:23]([O-:26])(=[O:25])=[O:24])[C:14]([CH:13]=[CH:12][C:9]2[C:8]([S:27]([O-:30])(=[O:29])=[O:28])=[CH:7][C:6]([N+:3]([O-:5])=[O:4])=[CH:11][CH:10]=2)=[CH:19][CH:18]=1)([O-:22])=[O:21].[K+:32].[K+:32]Participants
Conditions
- Temperature
- 70 °C
Procedure
1000 g of 4.5% strength by weight sodium hydroxide solution and 3 g of 4,4'-dinitrostilbene-2,2'-disulphonic acid are initially taken at 70° C. 124 g of 87.2% strength finely powdered 4,4'-dinitrodibenzyl-2,2'-disulphonic acid and 430 g of 6.19% strength by weight aqueous potassium hydroxide solution are added in small portions (approximately 20 portions) at 70° C. 50 l/hour of oxygen and 20 l/hour of air are passed into the reaction mixture for the whole duration of the experiment. After the mixture has been stirred for a further 2 hours at 70° C., a further 6 g of 100% strength by weight potassium hydroxide solution are added and the mixture is neutralized with 210 g of 30% strength by weight hydrochloric acid. 145 g of moist dipotassium 4,4'-dinitrostilbene-2,2'-disulphonate, corresponding to 124.7 g of dry material are isolated by filtration. The yield is found to be 97.2% of theory according to analysis by means of the HPLC method.
Workup
- customare initially taken at 70° C
Sources & evidence
- ORD record
- ord-54a93c1a5a61434a935afb3fa6f3316c
- Source dataset
- uspto-grants-1987_07
- Patent number
- US04680146
Linked notes
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