Hydrochloric Acid → HCID 13671877, Verbindung

HRID 1655322Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1655322
[NH2:1][CH:2]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[Cl:17][CH2:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.[ClH:27].C(OCC)(=O)C>C(O)C.CCCCCC>[ClH:17].[ClH:27].[C:5]1([CH:3]([OH:4])[CH:2]([NH:1][CH2:18][CH2:19][CH2:20][N:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 462682-Amino-1-phenyloctan-1-olHCID 79625Piperidine, 1-(3-chloropropyl)-

Produkt 1

HCID 13671877HCID 13671877, VerbindungAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8058HexaneLösungsmittel

Versuchsvorschrift

A mixture of (1RS,2RS)-2-amino-1-phenyloctan-1-ol (1.77 g, 8 mmol) and 1-(3-chloropropyl)piperidine (1.29 g, 8 mmol) was melted at 70° C. in a nitrogen atmosphere. The mixture was then heated at 110° to 120° C. for 3 hours. The reaction mixture was dissolved with heating in ethanol, followed by addition of concentrated hydrochloric acid (0.67 ml). Ethyl acetate was added and the resulting mixture was allowed to stand. Precipitated crystals were collected by filtration and washed with ethyl acetate and then with hexane to obtain 1.96 g of the title compound as white crystals (yield: 59%).

Aufarbeitung

  1. temperatureThe mixture was then heated at 110° to 120° C. for 3 hours
  2. dissolutionThe reaction mixture was dissolved
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration
  5. washwashed with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-33defaaa5d474bbdae105d28b5990846
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05250546

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