3-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazapine → 3-methoxy-11H-s-triazolo[3,4-b][3]benzazepine

HRID 26523Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 26523
CS([C:5]1[N:14]2[C:8]([CH2:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH:12]=[CH:13]2)=[N:7][N:6]=1)(=O)=O.[CH3:19][O-:20].[Na+].CO>CO>[CH3:19][O:20][C:5]1[N:14]2[C:8]([CH2:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH:12]=[CH:13]2)=[N:7][N:6]=1

Komponenten

4

Edukt 2

HCID 213235253-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazapineHCID 23694274Sodium methanolate methanol

Produkt 1

HCID 213233683-methoxy-11H-s-triazolo[3,4-b][3]benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To 0.522 g of 3-methylsulfonyl-11H-s-triazolo[3,4-b][3]benzazepine in 5 ml of methanol was added 3 ml of 2 N-sodium methoxide/methanol. The mixture was refluxed for 15 minutes and then the solvent was evaporated off. The residue was diluted with water and extracted with chloroform. The chloroform layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with isopropyl ether. By the above procedure was obtained 3-methoxy-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethyl acetate-n-hexane yielded colorless prisms, melting point: 160°-161° C.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 15 minutes
  2. customthe solvent was evaporated off
  3. additionThe residue was diluted with water
  4. extractionextracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialdried over Na2SO4
  7. customThe solvent was then evaporated off
  8. additionthe residue was treated with isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-a9d49ac76bfe42409466037a002bccaa
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150139

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