Hydrochloric Acid → HCID 13206062, compound

HRID 580190Notes

Reaction equation

HRID 580190 reaction equation
[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][N:3]=1.S(=O)(=O)(O)[OH:12].[OH-].[K+].Cl>O>[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([OH:12])[CH:9]=2)[NH:4][N:3]=1

Participants

6

Conditions

Temperature
80 °C

Procedure

A mixture consisting of 5 g of 3-aminoindazole and 4.3 g of 95% sulfuric acid was stirred for 3 hours at 80° C. To the mixture was added 13 ml of water, and the pH of the mixture was adjusted to 14 with potassium hydroxide. The mixture was washed twice with 20 ml of chloroform, and water was removed under reduced pressure. The residue thus obtained was added with 12.5 g of potassium hydroxide and 0.6 ml of water, and the mixture was stirred for 8 hours at 250° C. After cooling, to the mixture was added hydrochloric acid to separate crystals. The crystals were obtained by filtration and dried to give 2.86 g of 3-amino-5-hydroxyindazole having the following analytical values.

Workup

  1. washThe mixture was washed twice with 20 ml of chloroform, and water
  2. customwas removed under reduced pressure
  3. customThe residue thus obtained
  4. stirringthe mixture was stirred for 8 hours at 250° C
  5. temperatureAfter cooling, to the mixture
  6. customto separate crystals
  7. customThe crystals were obtained by filtration
  8. customdried

Sources & evidence

ORD record
ord-9dad9a9eb19d486898a966cfdaa2c08b
Source dataset
uspto-grants-1988_06
Patent number
US04751302

Reaction notes

Loading…