Acetic Acid → Aptazapine

HRID 1447399Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1447399
[CH3:1][N:2]1[C:19](=O)[C:18](=O)[N:5]2[C:6]3[CH:17]=[CH:16][CH:15]=[CH:14][C:7]=3[CH2:8][N:9]3[CH:13]=[CH:12][CH:11]=[C:10]3[CH:4]2[CH2:3]1.C(O)(=O)C>O1CCCC1.B#B>[CH3:1][N:2]1[CH2:19][CH2:18][N:5]2[C:6]3[CH:17]=[CH:16][CH:15]=[CH:14][C:7]=3[CH2:8][N:9]3[CH:13]=[CH:12][CH:11]=[C:10]3[CH:4]2[CH2:3]1

Komponenten

5

Edukt 2

HCID 176Acetic AcidHCID 128377152-methyl-3,4-dioxo-1,2,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine

Produkt 1

HCID 51355Aptazapine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittel2×HCID 6328200DiboronLösungsmittel

Versuchsvorschrift

To the suspension of 12.8 g of 2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine in 460 ml of tetrahydrofuran, 200 ml of 1-molar diborane in tetrahydrofuran are added while stirring and cooling with ice. The mixture is refluxed for one hour, again cooled and combined with 25 ml of acetic acid. It is evaporated, the residue taken up in 50 ml of 30% aqueous sodium hydroxide and the mixture extracted with methylene chloride. The extract is dried, evaporated, the residue dissolved in diethyl ether, the solution filtered and the filtrate evaporated, to yield the 2-methyl-1,3,4,14b-tetrahydro-10H--pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine.

Aufarbeitung

  1. additionare added
  2. temperaturecooling with ice
  3. temperatureThe mixture is refluxed for one hour
  4. temperatureagain cooled
  5. customIt is evaporated
  6. extractionthe mixture extracted with methylene chloride
  7. customThe extract is dried
  8. customevaporated
  9. dissolutionthe residue dissolved in diethyl ether
  10. filtrationthe solution filtered
  11. customthe filtrate evaporated

Quellen und Nachweise

ORD-Eintrag
ord-d76781500de2432aae5c7fd6185775b0
Quelldatensatz
uspto-grants-1982_02
Patentnummer
US04316900

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