Hydrogen Sulfide → HCID 178491226、化合物

HRID 490092ノート

反応式

HRID 490092 の反応式
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

参加物

5

反応物 4

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

生成物 1

HCID 178491226HCID 178491226、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-24d66aa78e084400a3003ed46a81d3c7
出典データセット
uspto-grants-2009_05
特許番号
US07528132B2

反応ノート

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