Water → HCID 23028102, compound

HRID 1946458Notes

Reaction equation

HRID 1946458 reaction equation
[CH2:1]([C:3]1[N:4]=[C:5]2[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[N:7][N:6]2[C:13]=1[S:14]([NH2:17])(=[O:16])=[O:15])[CH3:2].ClC1C=CC=C(C(OO)=O)C=1.[OH2:29].[OH2:30].N>CN(C=O)C>[CH2:1]([C:3]1[N:4]=[C:5]2[CH:10]=[CH:9][C:8]([S:11]([CH3:12])(=[O:30])=[O:29])=[N:7][N:6]2[C:13]=1[S:14]([NH2:17])(=[O:15])=[O:16])[CH3:2]

Participants

6

Reactant 4

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 12896473Azane;hydrateHCID 23028117HCID 23028117, compound

Product 1

HCID 23028102HCID 23028102, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

2-Ethyl-6-methylthioimidazo[1,2-b]pyridazin-3-ylsulfonamide (1.10 g, 4.04 mmol) was dissolved in DMF (10.0 ml) and stirred under ice-cooling, during which m-chloro-perbenzoic acid (abbreviated into mCPBA) (70%, 2.48 g, 10.1 mmol) was added thereto. The mixture was stirred under ice-cooling for 1 hour and at TOM temperature for 3 hours, and then the reaction solution was poured into water (50.0 ml), and 25% ammonia water (1.0 ml) was added thereto. After the reaction solution was stirred for 5 minutes, the precipitated crystals were filtered and washed with water, to give the title compound as colorless crystals. The yield was 1.04 g (84.5%).

Workup

  1. additionwas added
  2. stirringThe mixture was stirred under ice-
  3. temperaturecooling for 1 hour and at TOM temperature for 3 hours
  4. additionwas added
  5. stirringAfter the reaction solution was stirred for 5 minutes
  6. filtrationthe precipitated crystals were filtered
  7. washwashed with water

Sources & evidence

ORD record
ord-23b098f8748f49d88c0d93a3a802a198
Source dataset
uspto-grants-2013_03
Patent number
US08399381B2

Reaction notes

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