Water → HCID 54424979, compound

HRID 1416162Notes

Reaction equation

HRID 1416162 reaction equation
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].O.[N+:9]([C:12]1[CH:21]=[C:20]2[C:15]([NH:16][C:17](=[O:23])[C:18](=[O:22])[NH:19]2)=[CH:14][C:13]=1[S:24](Cl)(=[O:26])=[O:25])([O-:11])=[O:10]>>[OH:4][CH2:3][CH2:2][N:1]([CH2:5][CH2:6][OH:7])[S:24]([C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][C:12]=1[N+:9]([O-:11])=[O:10])[NH:19][C:18](=[O:22])[C:17](=[O:23])[NH:16]2)(=[O:25])=[O:26]

Participants

4

Reactant 3

HCID 962WaterHCID 8113DiethanolamineHCID 54433101HCID 54433101, compound

Product 1

HCID 54424979HCID 54424979, compoundYield 52%

Procedure

To a solution of 10,5 g (0.1 mole) of diethanolamine in 40 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 under stirring, the reaction mixture is stirred at room temperature for 6 hours and then allowed to stand for 16 hours. The separated crystals are filtered off, washed with water, dried and recrystallized from acetone. Thus 3.90 g (52%) of N,N-bis(2-hydroxyethyl)-1,2,3,4-tetrahydro-7-nitro-2,3-dioxo-6-quinoxaline sulfonamide are obtained, m.p.: 310-321° C.

Workup

  1. stirringthe reaction mixture is stirred at room temperature for 6 hours
  2. filtrationThe separated crystals are filtered off
  3. washwashed with water
  4. customdried
  5. customrecrystallized from acetone

Sources & evidence

ORD record
ord-39aadca5c6674a32a79156afd131fa31
Source dataset
uspto-grants-1999_06
Patent number
US05912245

Reaction notes

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