Diethyl Ether → HCID 10752374, Verbindung

HRID 345856Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 345856
[I-].[C:2]1([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][N+:9]=2[CH3:18])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:19](OCC)C.C[Mg]Br.[Cl-].[NH4+]>O1CCCC1.C(OCC)(=O)C>[CH3:19][C:8]1([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][N:9]1[CH3:18]

Komponenten

7

Edukt 4

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 10521731HCID 10521731, VerbindungHCID 178418573HCID 178418573, Verbindung

Produkt 1

HCID 10752374HCID 10752374, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a suspension of 1-phenyl-2-methyl-3,4-dihydroisoquinolinium iodide (1.0 g) in tetrahydrofuran (15 ml) was added 3M diethyl ether solution of methyl magnesium bromide (1.9 ml) with stirring at room temperature. After stirring for 30 minutes, the mixture was poured into saturated ammonium chloride aqueous solution and ethyl acetate. The organic layer was washed with water, sodium chloride aqueous solution and dried over magnesium sulfate, and evaporated in vacuo. The residue was recrystallized from n-hexane to give 1,2-dimethyl-1-phenyl-1,2,3,4-tetrahydroisoquinoline (0.6 g).

Aufarbeitung

  1. stirringAfter stirring for 30 minutes
  2. washThe organic layer was washed with water, sodium chloride aqueous solution
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was recrystallized from n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-6c1441b1ac2a4f198b360c0d349df31c
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05059608

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