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Hydrochloric Acid → HCID 178428593, compound

HRID 1898925
Notes
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Reaction equation

HRID 1898925 reaction equation
[ClH:1].[C:2]([C:4]([C:17](=[O:33])[N:18]([CH2:29][CH:30]1[CH2:32][CH2:31]1)[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)=[CH:5][NH:6][C:7](=[NH:16])[N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15])#[N:3]>O>[ClH:1].[C:2]([C:4]([C:17](=[O:33])[N:18]([CH2:29][CH:30]1[CH2:32][CH2:31]1)[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)=[CH:5][NH:6][C:7](=[NH:16])[N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15])#[N:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 178428592HCID 178428592, compound

Product 1

HCID 178428593HCID 178428593, compoundYield 94.9%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.5 ml of 2N HCl was added to a suspension of 449 mg (1 mmol) of the compound II obtained as in Example 85 in 2.5 ml of water at room temperature, and the mixture was stirred at room temperature for 10 minutes and while cooling in ice for 40 minutes and then filtered with suction. The crystals were dried over P4O10 in vacuo (6-8 mbar) at 23°-25° for 28 hours. 0.46 g (94.9% yield) of 1-cyano-1-[N-cyclopropylmethyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene hydrochloride was obtained, melting point 179°-180°.

Workup

  1. temperaturewhile cooling in ice for 40 minutes
  2. filtrationfiltered with suction
  3. dry with materialThe crystals were dried over P4O10 in vacuo (6-8 mbar) at 23°-25° for 28 hours

Sources & evidence

ORD record
ord-084bcc199b4942ae960c7a5afc921896
Source dataset
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05571816

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes