Hydrochloric Acid → 6-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride

HRID 1013095Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1013095
[CH3:1][O:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[ClH:14].CCCCCCC>C(O)C>[ClH:14].[CH3:1][O:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 8900HeptaneHCID 138533586-Methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

Produkt 1

HCID 574580206-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochlorideAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

Dissolve crude 6-methoxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (35.1 g, 0.198 mol) in ethanol (250 mL). Heat the solution to reflux and add 2 N HCl in ethanol (108.9 mL, 0.218 mol, 1.1 equiv.). Slowly add heptane (700 mL) over 10 min, then remove the heating mantle and cool the solution to RT and finally continue the cooling with an ice water mixture. Collect the resulting solid by vacuum filtration and wash with cold 1:2 ethanol:heptane (3×100 mL), dry for 15 min while applying vacuum suction, then further dry the product in a vacuum oven at 60° C. for 1 h to give the title compound as a white granular solid (35.53 g, 63%).

Aufarbeitung

  1. temperatureHeat the solution
  2. temperatureto reflux
  3. customremove the heating mantle
  4. customCollect the resulting solid
  5. filtrationby vacuum filtration
  6. washwash with cold 1:2 ethanol
  7. dry with materialheptane (3×100 mL), dry for 15 min
  8. customfurther dry the product in a vacuum oven at 60° C. for 1 h

Quellen und Nachweise

ORD-Eintrag
ord-42bd5e048db744538c1c8ac5a40e90de
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07981882B2

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