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Hydrochloric Acid → 1-Methyl-1,2,3,4-tetrahydroquinolin-8-amine

HRID 1866046
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1866046
Cl.[CH3:2][N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH:13]C(OC(C)(C)C)=O)[CH2:6][CH2:5][CH2:4]1>CO>[CH3:2][N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH2:13])[CH2:6][CH2:5][CH2:4]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 22708766HCID 22708766, Verbindung

Produkt 1

HCID 227087571-Methyl-1,2,3,4-tetrahydroquinolin-8-amineAusbeute 91,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Anhydrous HCl (gas) was bubbled through a stirred solution of 1-methyl-8-(N-tert-butoxycarbonylamino)-1,2,3,4-tetrahydroquinoline (0.83 g, 3.16 mmol) in methanol (30 mL), at room temperature, for 10 minutes. The resultant solution was stirred at room temperature for 1 hour then concentrated under reduced pressure. The residue was partitioned between CH2Cl2 (50 mL) and aqueous NaOH (10 N, 10 mL). The phases were separated and the aqueous phase was extracted with CH2Cl2 (3×10 mL). The combined organic extracts were dried (Na2SO4) and concentrated to afford 0.468 g (88%) of 1-methyl-8-amino-1,2,3,4-tetrahydroquinoline as a white solid. 1H NMR (CDCl3) δ 1.83-1.91 (m, 2H), 2.69 (s, 3H), 2.78 (t, 2H, J=6.6 Hz), 3.07-3.11 (m, 2H), 3.84 (br s, 2H, NH2), 6.52 (d, 1H, J=7.5 Hz), 6.56 (d, 1H, J=7.5 Hz), 6.81 (dd, 1H, J=7.5, 7.5 Hz).

Aufarbeitung

  1. concentrationthen concentrated under reduced pressure
  2. customThe residue was partitioned between CH2Cl2 (50 mL) and aqueous NaOH (10 N, 10 mL)
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with CH2Cl2 (3×10 mL)
  5. dry with materialThe combined organic extracts were dried (Na2SO4)
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-36a9d9b8eb294b11819b3553564cc0a6
Quelldatensatz
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07629337B2

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