Sodium Hydroxide → HCID 21611751, compound

HRID 358560Notes

Reaction equation

HRID 358560 reaction equation
C([O:3][C:4](=[O:20])[CH2:5][CH2:6][NH:7][C:8](=[S:19])[NH:9][C:10]1[CH:18]=[C:17]2[C:13]([CH:14]=[N:15][NH:16]2)=[CH:12][CH:11]=1)C.[OH-].[Na+]>CO.O>[NH:16]1[C:17]2[C:13](=[CH:12][CH:11]=[C:10]([NH:9][C:8]([NH:7][CH2:6][CH2:5][C:4]([OH:20])=[O:3])=[S:19])[CH:18]=2)[CH:14]=[N:15]1

Participants

5

Reactant 2

HCID 14798Sodium HydroxideHCID 53845013HCID 53845013, compound

Product 1

HCID 21611751HCID 21611751, compoundYield 56%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A solution of 0.6 g (2.05 mmol) of the ester thus obtained and 0.09 g (2.36 mmol) of sodium hydroxide in 15 ml of methanol and 0.1 ml of water is left at room temperature and under agitation for 20 hr. After concentration to dryness, 10 ml of water is added to the residue is obtained. After purification by extraction with ethyl acetate (3 × 20 ml), the aqueous phase is cooled and then acidified with a 3 N hydrochloric acid solution until a pH close to 3 is obtained 0.293 g (yield 56%) of (lH-indazol-6-yl)thiocarbamoyl-beta-alanine is obtained in the form of a solid having a melting point of 175° C.

Workup

  1. concentrationAfter concentration to dryness, 10 ml of water
  2. additionis added to the residue
  3. customis obtained
  4. customAfter purification
  5. extractionby extraction with ethyl acetate (3 × 20 ml)
  6. temperaturethe aqueous phase is cooled
  7. customa pH close to 3

Sources & evidence

ORD record
ord-94f9666de4e74f499c5f4b79fcb488b5
Source dataset
uspto-grants-1991_03
Patent number
US04997667

Reaction notes

Loading…