Hydrochloric Acid → HCID 67768990, Verbindung

HRID 1898913Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1898913
[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]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 3086669Opanixil

Produkt 1

HCID 67768990HCID 67768990, VerbindungAusbeute 92,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-2fbe8d7b3297448b9d2576725e81a436
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05571816

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