Methyl iodide → 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

HRID 26508

Reaktionsgleichung

Reaktionsgleichung von HRID 26508
[N:1]1[NH:2][C:3](=[S:15])[N:4]2[CH:10]=[CH:9][C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[CH2:6][C:5]=12.[CH3:16][O-].[Na+].CO.CI>CO>[CH3:16][S:15][C:3]1[N:4]2[C:5]([CH2:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[CH:10]2)=[N:1][N:2]=1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 130724232,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thioneHCID 23694274Sodium methanolate methanol

Produkt 1

HCID 213234063-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To 3 ml of methanol was added 0.215 g of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione and, under stirring, 0.6 ml of 2N-sodium methoxide/methanol was added. Then, 0.07 ml of methyl iodide was added dropwise. After 20 minutes, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with ether. In this manner, 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine were obtained as crystals. Recrystallization from methanol yielded colorless needles melting at 168°-169° C. This was identical with the products obtained in Examples 1 and 2.

Aufarbeitung

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over Na2SO4
  4. customThe solvent was then evaporated off
  5. additionthe residue was treated with ether

Quellen und Nachweise

ORD-Eintrag
ord-bab0281336fd44af883de71d8461ae1f
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150139

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