Hydrochloric Acid → HCID 178479552, compound

HRID 384234Notes

Reaction equation

HRID 384234 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][C:3]=1[NH:12][C:13](=[O:32])[NH:14][C:15]1[CH:16]=[C:17]([CH:28]=[C:29]([F:31])[CH:30]=1)[CH2:18][NH:19][C:20]1[C:21]([C:25]([NH2:27])=[O:26])=[N:22][NH:23][CH:24]=1.[ClH:33]>C(O)C.C(OCC)C>[ClH:33].[F:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:5]=[CH:4][C:3]=1[NH:12][C:13](=[O:32])[NH:14][C:15]1[CH:16]=[C:17]([CH:28]=[C:29]([F:31])[CH:30]=1)[CH2:18][NH:19][C:20]1[C:21]([C:25]([NH2:27])=[O:26])=[N:22][NH:23][CH:24]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 178513849HCID 178513849, compound

Product 1

HCID 178479552HCID 178479552, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 3283Diethyl EtherSolvent2×

Procedure

A suspension of 1.85 g (0.40 mmol) of 4-{3-[3-(2-fluoro-4-trifluoromethylphenyl)ureido]-5-fluorobenzylamino}-1H-pyrazole-3-carboxamide in 40 ml of ethanol is stirred at ambient temperature under an argon atmosphere. Then 20 ml (40 mmol) of a solution of hydrochloric acid in diethyl ether (1 N) are added dropwise. The reaction medium becomes a clear solution. After stirring for 12 hours at ambient temperature, the solvents are evaporated using a rotary evaporator under reduced pressure. The residue obtained is stirred in 200 ml of diethyl ether for 30 minutes.

Workup

  1. stirringAfter stirring for 12 hours at ambient temperature
  2. customthe solvents are evaporated
  3. customa rotary evaporator under reduced pressure
  4. customThe residue obtained

Sources & evidence

ORD record
ord-3dfbd33a10ad470e868d43aee3dde903
Source dataset
uspto-grants-2013_02
Patent number
US08367715B2

Reaction notes

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