Sulfur → 4,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

HRID 1606437Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1606437
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[O:13])[C:4]2[CH2:14][S:15][CH2:16][C:3]1=2.[S]>C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[O:13])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12

Komponenten

4

Edukt 2

HCID 5362487SulfurHCID 125216321,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b] [1,5]benzodiazepin-10-one

Produkt 1

HCID 125216424,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A mixture of 0.5 g. of 1,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b] [1,5]benzodiazepin-10-one and 0.5 g. of sulfur is fused at 160°C. ± 5 for 1 hour. The fusion mixture is slurried with chloroform and filtered. The filtrate is chromatographed on silica gel with benzene:methanol 9:1 to give a solid, which is recrystallized from methanol-water to give a tan solid, m.p. 224°-225°C. (dec.).

Aufarbeitung

  1. additionA mixture of 0.5 g
  2. filtrationfiltered
  3. customThe filtrate is chromatographed on silica gel with benzene:methanol 9:1
  4. customto give a solid, which
  5. customis recrystallized from methanol-water
  6. customto give a tan solid, m.p. 224°-225°C. (dec.)

Quellen und Nachweise

ORD-Eintrag
ord-82042532b08d4174acec56424b6c669b
Quelldatensatz
uspto-grants-1976_04
Patentnummer
US03953430

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