Acetic Acid → HCID 178427219, compound

HRID 503175Notes

Reaction equation

HRID 503175 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:16]3[C:11](=[C:12]([CH3:19])[CH:13]=C(C#N)[CH:15]=3)[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:20]([OH:23])(=[O:22])[CH3:21].S(=O)(=O)(O)O>O>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:16]3[C:11](=[C:12]([CH3:19])[CH:13]=[C:21]([C:20]([OH:23])=[O:22])[CH:15]=3)[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 178426383HCID 178426383, compound

Product 1

HCID 178427219HCID 178427219, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
100 °C

Procedure

To 430 mg of 3-(3-fluorophenyl)-7-methyl-1H-indazole-5-carbonitrile were sequentially added 6.0 ml of glacial acetic acid, 2.0 ml of water and 2.0 ml of concentrated sulfuric acid, followed by stirring at 100° C. for one day. After standing to cool, the reaction mixture was diluted with 20 ml of water, and the resulting crystals were collected by filtration. The crystals were sequentially washed with water and diethyl ether, to give 360 mg of the title compound as colorless crystals.

Workup

  1. temperatureto cool
  2. filtrationthe resulting crystals were collected by filtration
  3. washThe crystals were sequentially washed with water and diethyl ether

Sources & evidence

ORD record
ord-cfc90c4e239c4b6ba9cfd3e2e00e20f8
Source dataset
uspto-grants-2010_08
Patent number
US07776890B2

Reaction notes

Loading…