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HCID 21923071, Verbindung → HCID 178478851, Verbindung

HRID 1272661
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1272661
[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:33]=[CH:32][C:28]([C:29]([NH2:31])=[O: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]([NH2:31])=[O:30])=[CH:32][CH:33]=3)[N:11]=2)[CH2:4][CH2:3]1
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Komponenten

4

Edukt 2

HCID 21923071HCID 21923071, VerbindungHCID 178511674HCID 178511674, Verbindung

Produkt 1

HCID 178478851HCID 178478851, VerbindungAusbeute 116,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

The operation is carried out as in Stage 2 of Example 6 and 800 mg of trans-1,4-diaminocyclohexane is introduced at ambient temperature under agitation then the reaction medium is heated at approximately 150° C. until melting and 249 mg of the product obtained in Stage 1 above is added, the reaction medium is left under agitation for 4 hours 30 minutes then left to return to ambient temperature. Then 10 ml of water is added, followed by extracting with 10 ml of methylene chloride containing 25% of methanol, drying, filtering, evaporating to dryness and taking up in 5 ml of ethanol. 2 ml of 1.4 N HCl in ethanol is added, followed by evaporating, leaving to crystallize, separating and washing with ethanol then drying at a temperature of approximately 60° C. In this way 207 mg of expected product is obtained in the form of colourless crystals.

Aufarbeitung

  1. additionis introduced at ambient temperature under agitation
  2. waitthen left
  3. customto return to ambient temperature
  4. extractionby extracting with 10 ml of methylene chloride containing 25% of methanol
  5. customdrying
  6. filtrationfiltering
  7. customevaporating to dryness
  8. addition2 ml of 1.4 N HCl in ethanol is added
  9. customby evaporating
  10. customleaving
  11. customto crystallize
  12. customseparating
  13. washwashing with ethanol
  14. customthen drying at a temperature of approximately 60° C

Quellen und Nachweise

ORD-Eintrag
ord-c936872deef543dca63124b424d6f6cd
Quelldatensatz
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07208598B2

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