Methane → HCID 86749076, Verbindung

HRID 2211139

Reaktionsgleichung

Reaktionsgleichung von HRID 2211139
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:12][C:11]([CH:13]=[N:14][N:15]3[CH2:19][C:18](=[O:20])[N:17]([CH2:21][CH2:22][CH2:23][CH2:24][N:25]4[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27][CH2:26]4)[C:16]3=[O:32])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38]>CO>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38].[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]\[C:37]([OH:39])=[O:38].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[O:12][C:11]([CH:13]=[N:14][N:15]3[CH2:19][C:18](=[O:20])[N:17]([CH2:21][CH2:22][CH2:23][CH2:24][N:25]4[CH2:26][CH2:27][N:28]([CH3:31])[CH2:29][CH2:30]4)[C:16]3=[O:32])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 297MethaneHCID 609391-[(E)-[5-(4-chlorophenyl)furan-2-yl]methylideneamino]-3-[4-(4-methylpiperazin-1-yl)butyl]imidazolidine-2,4-dioneHCID 444266Maleic Acid

Produkt 1

HCID 86749076HCID 86749076, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

The free base compound, 1-[[[5-(4-chlorophenyl)-2-furanyl]methylene]amino]-3-[4-(4-methyl-1-piperazinyl)butyl]-2,4-imidazolidinedione [prepared as described in Example G herein], (4.4 g, 0.0096 mole) is dissolved in MeOH (125 ml), treated with activated charcoal, and filtered. To this solution is added a solution of maleic acid (2.23 g, 0.0192 mole) in one portion. The resulting mixture is stirred at room temperature for approximately 2 hours and is then collected, and air-dried. This solid is recrystallized from absolute EtOH/H2O (activated charcoal), filtered then cooled. The solid is collected, washed with anhydrous ether, air-dried and dried at 70° C. to give 4.99 g (0.0072 mole) of 1-[[[5-(4-chlorophenyl)-2-furanyl]methylene]amino]-3-[4-(4-methyl-1-piperazinyl)butyl]-2,4-imidazolidinedione di-2-Z-butenedioic acid salt.

Aufarbeitung

  1. filtrationfiltered
  2. customis then collected
  3. customair-dried
  4. customThis solid is recrystallized from absolute EtOH/H2O (activated charcoal)
  5. filtrationfiltered
  6. temperaturethen cooled
  7. customThe solid is collected
  8. washwashed with anhydrous ether
  9. customair-dried
  10. customdried at 70° C.

Quellen und Nachweise

ORD-Eintrag
ord-a2b502f89b8c4442aba651dcf8dc2a77
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05462940

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