Water → HCID 54430977, compound
Reaction equation
[CH3:1][O:2][CH2:3][CH2:4][NH2:5].O.[N+:7]([C:10]1[CH:19]=[C:18]2[C:13]([NH:14][C:15](=[O:21])[C:16](=[O:20])[NH:17]2)=[CH:12][C:11]=1[S:22](Cl)(=[O:24])=[O:23])([O-:9])=[O:8]>>[CH3:1][O:2][CH2:3][CH2:4][NH:5][S:22]([C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:10]=1[N+:7]([O-:9])=[O:8])[NH:17][C:16](=[O:20])[C:15](=[O:21])[NH:14]2)(=[O:23])=[O:24]Participants
4
Procedure
To a solution of 3.76 g (0.05 mole) of 2-methoxyethylamine in 15 ml of water 6.11 g (0.02 mole) of 1,2,3,4-tetrahydro-7-nitro-2,3-dioxo-6-quinoxalinesulfonyl chloride are added at room temperature, under stirring. The mixture is stirred at room temperature for 6 hours and then allowed to stand for 16 hours. The separated crystals are filtered off, washed successively with water and acetone, filtered again, dried and dissolved in a slight amount of hot dimethyl sulfoxide. The product is precipitated from this solution with water. Thus 4.05 g (59%) of 1,2,3,4-tetrahydro-N-(2-methoxy-ethyl)-7-nitro-2,3-dioxo-6-quinoxaline sulfonamide are obtained, m.p.: 320-321° C.
Workup
- stirringThe mixture is stirred at room temperature for 6 hours
- filtrationThe separated crystals are filtered off
- washwashed successively with water and acetone
- filtrationfiltered again
- customdried
- dissolutiondissolved in a slight amount of hot dimethyl sulfoxide
- customThe product is precipitated from this solution with water
Sources & evidence
- ORD record
- ord-206c15ded7914c40bf7f4bb9fe64234b
- Source dataset
- uspto-grants-1999_06
- Patent number
- US05912245
Reaction notes
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