Sodium Hydroxide → HCID 19083177, compound

HRID 963671Notes

Reaction equation

HRID 963671 reaction equation
[NH2:1]OS(O)(=O)=O.[OH-].[Na+].[Cl:9][C:10]1[C:11]2[C:15]([CH:16]=[CH:17][CH:18]=1)=[N:14][N:13]([CH3:19])[C:12]=2[S:20]([O-:22])=[O:21].[Li+]>O>[Cl:9][C:10]1[C:11]2[C:15]([CH:16]=[CH:17][CH:18]=1)=[N:14][N:13]([CH3:19])[C:12]=2[S:20]([NH2:1])(=[O:22])=[O:21]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 76284hydroxylamine-O-sulfonic acidHCID 23675696HCID 23675696, compound

Product 1

HCID 19083177HCID 19083177, compoundYield 69.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

45.2 g (0.4 mol) of hydroxylamine-O-sulfonic acid was gradually added to a solution containing 16 g (0.4 mol) of sodium hydroxide in water (300 ml) under cooling with ice (<10° C.). This solution was added all at once to a solution of the previously prepared crude lithium 4-chloro-2-methyl-2H-indazole-3-sulfinate in water (100 ml). The mixture was stirred at room temperature for 12 hours. Formed crystals were collected by filtration to obtain 17.1 g (yield: 69.8%) of the desired 4-chloro-2-methyl-2H-indazole-3-sulfonamide (slightly yellow granular crystals). Melting point: 173°-175° C.

Workup

  1. temperatureunder cooling with ice (<10° C.)
  2. additionThis solution was added all at once to a solution of the
  3. customFormed crystals
  4. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-819403e4807b45a382ab803066b682cc
Source dataset
uspto-grants-1998_06
Patent number
US05763616

Reaction notes

Loading…