Hydrochloric Acid → HCID 67913269, compound

HRID 345508Notes

Reaction equation

HRID 345508 reaction equation
Cl.[CH2:2]([O:6][C:7](=[O:24])[CH2:8][C:9]1[C:10]([N:21]([CH3:23])[CH3:22])=[N:11][NH:12][C:13]=1[C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)[CH2:3]CC.Cl>C(O)C>[ClH:20].[CH2:2]([O:6][C:7](=[O:24])[CH2:8][C:9]1[C:10]([N:21]([CH3:22])[CH3:23])=[N:11][NH:12][C:13]=1[C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)[CH3:3]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 67913259HCID 67913259, compound

Product 1

HCID 67913269HCID 67913269, compoundYield 120.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 5.6 g (0.015 mole) of 5-(4-chlorophenyl)-3-dimethylamino-1H-pyrazole-4-acetic acid butyl ester monohydrochloride in 150 ml of 200 ethanol was treated with 1 ml of concentrated hydrochloric acid and heated at reflux for 24 hours. The reaction mixture was concentrated in vacuo to a solid residue, 5.5 g. Recrystallization from 2-propanol yielded 3.1 g (60%) of white crystalline product, mp 211°-215° C. with degassing.

Workup

  1. temperatureheated
  2. temperatureat reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated in vacuo to a solid residue, 5.5 g
  4. customRecrystallization from 2-propanol

Sources & evidence

ORD record
ord-12d4147ab8c147ceb3fe1989a6c70a1b
Source dataset
uspto-grants-1991_10
Patent number
US05057534

Reaction notes

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