Hydrochloric Acid → HCID 67768990, compound

HRID 1898913Notes

Reaction equation

HRID 1898913 reaction equation
[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]>CCOCC.CC(C)=O>[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:29])[F:30])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 3086669Opanixil

Product 1

HCID 67768990HCID 67768990, compoundYield 92.7%

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 3283Diethyl EtherSolvent

Procedure

1.52 ml of a 6.6 molar solution of HCl in ether were added dropwise to a solution of 3.80 g (9 mmol) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)-pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide prepared as in Example 1 in 20 ml of acetone at room temperature, and the resulting suspension was stirred while cooling in ice for 20 minutes. The crystals were then filtered off with suction, washed with acetone and ether and dried in vacuo (6-7 mbar) at 100° for 10 hours. 3.83 g (=92.7% yield) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide hydrochloride were obtained, melting point 264°-265° (decomposition).

Workup

  1. temperaturewhile cooling in ice for 20 minutes
  2. filtrationThe crystals were then filtered off with suction
  3. washwashed with acetone and ether
  4. customdried in vacuo (6-7 mbar) at 100° for 10 hours

Sources & evidence

ORD record
ord-2fbe8d7b3297448b9d2576725e81a436
Source dataset
uspto-grants-1996_11
Patent number
US05571816

Reaction notes

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