Dimethylamine → HCID 9400787, compound

HRID 655617Notes

Reaction equation

HRID 655617 reaction equation
Cl[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH3:14]>>[CH3:12][N:13]([CH3:14])[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1

Participants

3

Reactant 2

HCID 674DimethylamineHCID 12015126-chloropyridine-3-sulfonamide

Product 1

HCID 9400787HCID 9400787, compoundYield 95%

Procedure

A mixture of 6-chloropyridine-3-sulfonamide (5 g, 0.0259 mol) and aqueous dimethylamine (100 ml, 40%) is stirred at rt for 13 h. The mixture is concentrated to ⅕th of its original volume and cooled. The precipitate is collected by filtration, washed with ice-cold water (10 ml) and dried under vacuum to afford 4.5 g (95%) of the title compound as a solid. mp: 133-138° C., LC/MS: (ES+) 201.9.

Workup

  1. concentrationThe mixture is concentrated to ⅕th of its original volume
  2. temperaturecooled
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with ice-cold water (10 ml)
  5. customdried under vacuum

Sources & evidence

ORD record
ord-c6187a94f133448eb1d446df590dd669
Source dataset
uspto-grants-2011_12
Patent number
US08071597B2

Reaction notes

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