Hydrogen Sulfide → HCID 178491226, Verbindung

HRID 490092Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 490092
C(C1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8](CC1C=CC(OC)=CC=1)[N:7]=[C:6]2[CH3:21])#N.C([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])C.N1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.[SH2:35].C([O:39][CH2:40]C)(=O)C>>[CH3:40][O:39][C:32]1[CH:33]=[CH:34][C:28]([CH2:27][N:24]=[C:25]([C:26]2[CH:4]=[C:5]3[C:9](=[CH:10][CH:11]=2)[NH:8][N:7]=[C:6]3[CH3:21])[SH:35])=[CH:30][CH:31]=1

Komponenten

5

Edukt 4

HCID 402Hydrogen SulfideHCID 8857Ethyl AcetateHCID 22561186Pyridine triethylamineHCID 689992085-cyano-N-(4-methoxybenzyl)-3-methylindazole

Produkt 1

HCID 178491226HCID 178491226, Verbindung

Versuchsvorschrift

To a solution of 5-cyano-N-(4-methoxybenzyl)-3-methylindazole 106 (0.25 g, 0.903 mmol) in 10% v/v triethylamine-pyridine (10 mL) was bubbled hydrogen sulfide gas for 10 minutes. The reaction mixture was stirred at room temperature for 16 hours. Ethyl acetate (100 mL) was added and the organic layer was washed with water, 1% aqueous citric acid and brine. The organic layer was dried over sodium sulfate. The organic solvent was evaporated under reduced pressure to yield N-(4-methoxybenzyl)-3-methylindazole-5-carboximidothioic acid 107 which was used in the next step without further purification.

Aufarbeitung

  1. washthe organic layer was washed with water, 1% aqueous citric acid and brine
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customThe organic solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-24d66aa78e084400a3003ed46a81d3c7
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07528132B2

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