Ammonium Hydroxide → 1-Methyl-7-nitro-3,4-dihydroisoquinoline

HRID 369982

Reaktionsgleichung

Reaktionsgleichung von HRID 369982
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+].[OH-].[NH4+]>>[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[CH2:5][CH2:4][N:3]=1

Komponenten

4

Edukt 3

HCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 2315021-Methyl-3,4-dihydroisoquinoline

Produkt 1

HCID 109322281-Methyl-7-nitro-3,4-dihydroisoquinoline

Versuchsvorschrift

1-Methyl-3,4-dihydroisoquinoline (4.25 g, 29.3 mmol) was dissolved in ice cold concentrated sulfuric acid (15 ml) and to this was added potassium nitrate (3.25 g, 32.2 mmol) portionwise with cooling. The mixture was stirred overnight, poured over ice, basified with concentrated ammonium hydroxide, and the precipitated solid was collected, washed with water and dried: 4.47 g (80%), MS (M+H)+ 191, 1H NMR (D2O), 8.30 (d, 1H), 8.22 (dd, 1H), 7.39 (d, 1H), 3.80-3.62 (m, 2H), 2.92-2.70 (m, 2H), 2.48 (broad s, 3H).

Aufarbeitung

  1. temperaturewith cooling
  2. additionpoured over ice
  3. customthe precipitated solid was collected
  4. washwashed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-5cffc12037354434a37b3a773f26cd97
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06140322

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