Hydrochloric Acid → HCID 178485721, compound

HRID 482264Notes

Reaction equation

HRID 482264 reaction equation
[ClH:1].[C:2]([C:4]([C:17](=[O:30])[N:18]([CH3:29])[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]>CCOCC.C(O)C>[ClH:1].[C:2]([C:4]([C:17](=[O:30])[N:18]([CH3:29])[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:26])([F:27])[F:28])[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]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 178485720HCID 178485720, compound2×

Product 1

HCID 178485721HCID 178485721, compoundYield 90.7%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 3283Diethyl EtherSolvent

Procedure

3.1 ml of a 6.6 molar solution of HCl in ether were added dropwise to a suspension of 8.17 g (20 mmol) of 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]-ethene (compound IV) in 48 ml of ethanol at room temperature, and the mixture was stirred at 1°-3° C. for 1 hour. The solid was then filtered off with suction, washed with ether and dried at room temperature in vacuo (4-6 mbar) for 20 hours. 8.34 g (=90.7% yield) of pure 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino-(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene hydrochloride were obtained, melting point 180°-181° C. (=transition point; substance resolidifies); C18H20ClF3N6O2 (444.86)

Workup

  1. filtrationThe solid was then filtered off with suction
  2. washwashed with ether
  3. customdried at room temperature in vacuo (4-6 mbar) for 20 hours

Sources & evidence

ORD record
ord-6a1e8720a3834f7c8cdd69406e8f0570
Source dataset
uspto-grants-1998_08
Patent number
US05795899

Reaction notes

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