Chlorosulfonic acid → HCID 178434314, compound

HRID 1786655Notes

Reaction equation

HRID 1786655 reaction equation
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH3:6][C:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9](C(=O)C)[N:8]=1>>[CH3:6][C:7]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:14]=2)[NH:9][N:8]=1

Participants

3

Reactant 2

HCID 24638Chlorosulfonic acidHCID 126391861-(3-methyl-1H-indazol-1-yl)Ethanone

Product 1

HCID 178434314HCID 178434314, compoundYield 63.6%

Procedure

To chlorosulfonic acid (0.38 ml, 5.7 mmol) under a blanket of argon in an ice bath was added 1-(3-methyl-indazol-1-yl)-ethanone (200 mg, 1.1 mmol). The reaction was allowed to warm to RT and then was heated at 70° C. for 45 min. The reaction was cooled to rt, slowly quenched over ice and extracted with dichloromethane. The organic phase was dried over MgSO4 and concentrated in vacuo to a tan solid (160 mg, 0.7 mmol, 61% yield).

Workup

  1. temperaturewas heated at 70° C. for 45 min
  2. temperatureThe reaction was cooled to rt
  3. customslowly quenched over ice
  4. extractionextracted with dichloromethane
  5. dry with materialThe organic phase was dried over MgSO4

Sources & evidence

ORD record
ord-838c87c92f474128935a7992ddabd067
Source dataset
uspto-grants-2009_03
Patent number
US07507763B2

Reaction notes

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