HCID 21923039, Verbindung → HCID 178478686, Verbindung

HRID 1244948Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1244948
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]1.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[CH:15][N:16]2[CH:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)=[C:12]([NH:24][C:25]2[CH:32]=[CH:31][C:28]([C:29]#[N:30])=[CH:27][CH:26]=2)[N:11]=1>O>[ClH:9].[ClH:9].[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:10]2[N:18]=[C:17]3[C:13]([N:14]=[CH:15][N:16]3[CH:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)=[C:12]([NH:24][C:25]3[CH:26]=[CH:27][C:28]([C:29]#[N:30])=[CH:31][CH:32]=3)[N:11]=2)[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 21923039HCID 21923039, VerbindungHCID 178511674HCID 178511674, Verbindung

Produkt 1

HCID 178478686HCID 178478686, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

2 g of trans-1,4-diaminocyclohexane is taken to approximately 150° C. then 1.18 g of the product obtained in Stage 1 above is added, the reaction medium is maintained under agitation to 140° C. for 6 hours then left to return to ambient temperature. Then 30 ml of water is added, followed by extracting with dichloromethane, drying and evaporating the solvent. The residue is chromatographed on silica (eluent: MeOH/NH4OH 98/2), 130 mg of the product obtained is removed and taken up in 10 ml of ethanol, 4 ml of an ethanolic solution of hydrochloric acid is added, followed by separating, washing with ether, drying under reduced pressure at 50° C. and 144 mg of expected product is recovered.

Aufarbeitung

  1. customis taken to approximately 150° C.
  2. waitthen left
  3. customto return to ambient temperature
  4. extractionby extracting with dichloromethane
  5. customdrying
  6. customevaporating the solvent
  7. customThe residue is chromatographed on silica (eluent: MeOH/NH4OH 98/2), 130 mg of the product
  8. customobtained
  9. customis removed
  10. addition4 ml of an ethanolic solution of hydrochloric acid is added
  11. customby separating
  12. washwashing with ether
  13. customdrying under reduced pressure at 50° C.
  14. custom144 mg of expected product is recovered

Quellen und Nachweise

ORD-Eintrag
ord-1f26b40f5202410ab618aae20ec0dc98
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07122669B1

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