Ethanol → HCID 178423444、化合物

HRID 916082ノート

反応式

HRID 916082 の反応式
[C:1]1([CH2:11][NH:12][C:13]2[CH:18]=C[C:16](C)=[CH:15][C:14]=2[NH2:20])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[SH-:21].[C+4:22].[SH-].[SH-].[SH-].[CH2:26](O)[CH3:27]>>[C:1]1([CH2:11][N:12]2[C:13]3[CH:18]=[C:26]([CH3:27])[CH:16]=[CH:15][C:14]=3[N:20]=[C:22]2[SH:21])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 3

HCID 702EthanolHCID 17810729((1-Naphthyl)methyl)(2-amino-4-methyl-phenyl)amineHCID 178420937HCID 178420937、化合物

生成物 1

HCID 178423444HCID 178423444、化合物収率 44%

実験手順

Subsequently, ((1-naphthyl)methyl)(2-amino-4-methyl-phenyl)amine (943.1 mg, 3.59 mmol) was dissolved in ethanol (6.4 ml), to which carbon bisulfide (7 ml, 116 mmol) was added, and then refluxed. After 10 hours, it was returned to room temperature, concentrated under reduced pressure. Ethanol (2 ml) was added to the residue, which was stirred at room temperature for 30 minutes, and was further stirred on ice for 30 minutes. The resulting crystals were filtered, and dried to obtain 1-((1-naphthyl)methyl)-6-methyl-benzimidazole-2-thiol (459.1 mg, yield 44%, 2 steps).

後処理

  1. additionwas added
  2. temperaturerefluxed
  3. customwas returned to room temperature
  4. concentrationconcentrated under reduced pressure
  5. additionEthanol (2 ml) was added to the residue, which
  6. stirringwas further stirred on ice for 30 minutes
  7. filtrationThe resulting crystals were filtered
  8. customdried

出典と根拠

ORDレコード
ord-24e62a9e4c214738bfaf1dc9e2a399eb
出典データセット
uspto-grants-2007_09
特許番号
US07268145B2

反応ノート

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