Formic Acid → 6-Chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 971612Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 971612
[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][NH:9][CH2:8][CH:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:5]=[C:4]([O:19][CH3:20])[C:3]=1[O:21][CH3:22].[OH-].[Na+].[CH:25](O)=O>C=O>[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][N:9]([CH3:25])[CH2:8][CH:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:5]=[C:4]([O:19][CH3:20])[C:3]=1[O:21][CH3:22]

Komponenten

5

Edukt 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 12668015HCID 12668015, Verbindung

Produkt 1

HCID 4359706-Chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 712FormaldehydeLösungsmittel

Versuchsvorschrift

A solution of 3.7 g of 6-chloro-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine in 15 ml of formic acid and 10 ml of formaldehyde is refluxed for 18 hours. The reaction mixture is evaporated to dryness, 20 ml of 6N hydrochloric acid is added and the solution is again evaporated to dryness to give a liquid. The latter is treated with 20 ml of 10% sodium hydroxide solution and the mixture is extracted with ether. The dried extract is evaporated to give 6-chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine.

Aufarbeitung

  1. customThe reaction mixture is evaporated to dryness, 20 ml of 6N hydrochloric acid
  2. additionis added
  3. customthe solution is again evaporated to dryness
  4. customto give a liquid
  5. extractionthe mixture is extracted with ether
  6. extractionThe dried extract
  7. customis evaporated

Quellen und Nachweise

ORD-Eintrag
ord-536100f5df4f4cb1a94ee60a712b0aeb
Quelldatensatz
uspto-grants-1979_07
Patentnummer
US04160765

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