Formaldehyde → Sch-12679

HRID 596630Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 596630
[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[CH2:22]=O>C(O)=O>[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][N:9]([CH3:22])[CH2:10][CH2:11][C:5]=2[CH:4]=1

Komponenten

4

Edukt 2

HCID 712FormaldehydeHCID 105409631H-3-Benzazepine, 2,3,4,5-tetrahydro-7,8-dimethoxy-1-phenyl-

Produkt 1

HCID 5024Sch-12679

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 284Formic AcidLösungsmittel

Versuchsvorschrift

A solution of 3.58 g. (0.0126 mol) of 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 the liquid 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
  2. additionof 6N hydrochloric acid is added
  3. customthe solution is again evaporated to dryness
  4. customto give a liquid
  5. additionThe latter is treated with 20 ml
  6. extractionof 10% sodium hydroxide solution and the mixture is extracted with ether
  7. extractionThe dried extract
  8. customis evaporated

Quellen und Nachweise

ORD-Eintrag
ord-3c311c32b51e48cd9d32d7f1330e5a30
Quelldatensatz
uspto-grants-1977_03
Patentnummer
US04011319

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