Ammonia → RO-05-2921

HRID 1973070

Reaktionsgleichung

Reaktionsgleichung von HRID 1973070
C=O.[NH3:3].Cl[CH2:5][C:6]([NH:8][C:9]1[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=1[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=O)=[O:7]>CO>[C:13]1([C:11]2[C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]=3[NH:8][C:6](=[O:7])[CH2:5][N:3]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

5

Edukt 3

HCID 222Ammonia3×HCID 712FormaldehydeHCID 2064069N-(2-benzoylphenyl)-2-chloroacetamide

Produkt 1

HCID 76175RO-05-2921Ausbeute 84,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Paraformaldehyde (200 g., 91% flake) is placed in a stirred reactor equipped with a reflux condenser, decanter, and ammonia addition tube. Methanol (575 mls.) is added and then gaseous ammonia below the surface of the reaction mixture. 2-Chloroacetamido-benzophenone (273.7 g.) is then added. With a slow, continuous flow of ammonia to the reaction zone, the mixture is heated at reflux for 5 hours. The crystal slurry obtained is distilled to recover the methanol. Toluene (1350 mls.) is now added to the crystal residue and residual water is removed by azeotropic distillation through the decanter. When dry, the hot toluene solution is filtered, the filtrate is cooled for crystallization, and the product obtained isolated to give 1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (200 g., 84.7%) m.p. 180°-181° C. (uncorr.).

Aufarbeitung

  1. customequipped with a reflux condenser
  2. temperatureat reflux for 5 hours
  3. customThe crystal slurry obtained
  4. distillationis distilled
  5. customto recover the methanol
  6. additionToluene (1350 mls.) is now added to the crystal residue and residual water
  7. customis removed by azeotropic distillation through the decanter
  8. customWhen dry
  9. filtrationthe hot toluene solution is filtered
  10. temperaturethe filtrate is cooled for crystallization
  11. customthe product obtained
  12. customisolated

Quellen und Nachweise

ORD-Eintrag
ord-4caa97eb1a444f299db8130eb2318f7b
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03996209

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