Hydrochloric Acid → HCID 19961156, Verbindung

HRID 1089009Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1089009
[NH2:1][CH2:2][C:3]1(O)[C:12]2[C:7](=[C:8]([O:15][CH3:16])[C:9]([O:13][CH3:14])=[CH:10][CH:11]=2)[CH2:6][CH:5]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:4]1.[ClH:24]>C(O)(C)C>[ClH:24].[NH2:1][CH2:2][C:3]1[C:12]2[C:7](=[C:8]([O:15][CH3:16])[C:9]([O:13][CH3:14])=[CH:10][CH:11]=2)[CH2:6][CH:5]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:4]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 19961233HCID 19961233, Verbindung

Produkt 1

HCID 19961156HCID 19961156, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

1 Aminomethyl-5,6-dimethoxy-1-hydroxy-3-phenyl-1,2,3,4-tetrahydro-naphthalene (11.5 g, 37 mmol), from Step 1, was heated at reflux temperature in 300 mL of isopropyl alcohol saturated with hydrochloric acid for 2 h. The resultant solution was concentrated and the solid residue was triturated with hot toluene to give 10.6 g (98% yield) of 1-aminomethyl-3,4-dihydro-5,6-dimethoxy-3-phenyl-naphthalene hydrochloride, m.p. 189.5°-190° C. 1H NMR (d6 -DMSO) delta 2.78 (dd, 1H), 3.11 (dd, 1H), 3.2-3.4 (m, 2H +H2O), 3.6 (s, 3H), 3.81 (s, 3H), 3.93 (d, 1H), 6.1 (d, 1H), 6.93 (d, 1H), 7.12 (d, 1H), 7.2-7.4 (m, 5H).

Aufarbeitung

  1. concentrationThe resultant solution was concentrated
  2. customthe solid residue was triturated with hot toluene

Quellen und Nachweise

ORD-Eintrag
ord-1e37e223403d45999a037c22104ab31e
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04963568

Notizen zur Reaktion

Wird geladen…