Water → HCID 18509241, compound

HRID 1356678Notes

Reaction equation

HRID 1356678 reaction equation
Cl.[O:2]([NH2:4])[CH3:3].[Cl:5][C:6]1[CH:7]=[C:8]([S:13](Cl)(=[O:15])=[O:14])[CH:9]=[CH:10][C:11]=1[Cl:12].O>N1C=CC=CC=1>[Cl:5][C:6]1[CH:7]=[C:8]([S:13]([NH:4][O:2][CH3:3])(=[O:14])=[O:15])[CH:9]=[CH:10][C:11]=1[Cl:12]

Participants

5

Reactant 3

HCID 962WaterHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 521874O-Methylhydroxylamine hydrochloride

Product 1

HCID 18509241HCID 18509241, compoundYield 95%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

To a suspension of methoxylamine hydrochloride (0.93 g (11.1 mmol)) in pyridine (5.0 ml), 3,4-dichlorobenzenesulfonyl chloride (2.73 g (11.1 mmol)) was added with stirring under cooling with ice and the resulting mixture was stirred for one hour under cooling with ice, and at room temperature for 18 hours. Water (50.0 ml) was then added to the reaction mixture to bring about separation of crystals. The crystals were filtered and washed with water to give 2.69 g (95%) of 3,4-dichloro-N-methoxybenzenesulfonamide as pale yellow crystals.

Workup

  1. additionwas added
  2. temperatureunder cooling with ice
  3. stirringthe resulting mixture was stirred for one hour
  4. temperatureunder cooling with ice
  5. customto bring about separation of crystals
  6. filtrationThe crystals were filtered
  7. washwashed with water

Sources & evidence

ORD record
ord-093612096cbf429dae4f9fd468291fbd
Source dataset
uspto-grants-2003_07
Patent number
US06586617B1

Reaction notes

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