Ethanol → HCID 178488032、化合物

HRID 273756

反応式

HRID 273756 の反応式
C(O)C.[C:4](=[S:6])=S.[NH2:7][C:8]1[CH:9]=[C:10]([O:15][CH3:16])[CH:11]=[CH:12][C:13]=1[NH2:14].[OH-].[Na+]>O>[SH:6][C:4]1[NH:7][C:8]2[CH:9]=[C:10]([O:15][CH3:16])[CH:11]=[CH:12][C:13]=2[N:14]=1

参加物

6

反応物 4

HCID 702EthanolHCID 6348Carbon DisulfideHCID 14798Sodium HydroxideHCID 1534044-Methoxy-o-phenylenediamine

生成物 1

HCID 178488032HCID 178488032、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

70 ml of ethanol and 15 ml of carbon disulfide were added to 2.6 g of 3,4-diaminoanisole and then a solution of 1.5 g of sodium hydroxide in 5 ml of water was added thereto. After heating with a water bath for 3.5 hours, the mixture was cooled with ice, filtered and then the solvent in the filtrate was distilled off under reduced pressure. The residue was dissolved in ethanol. The solution was filtrated to remove the insoluble matter and then the solvent in the filtrate was distilled off under reduced pressure. The residue was recrystallized from water-containing methanol to obtain 2.0 g of the titled compound (13).

後処理

  1. temperatureAfter heating with a water bath for 3.5 hours
  2. temperaturethe mixture was cooled with ice
  3. filtrationfiltered
  4. distillationthe solvent in the filtrate was distilled off under reduced pressure
  5. dissolutionThe residue was dissolved in ethanol
  6. filtrationThe solution was filtrated
  7. customto remove the insoluble matter
  8. distillationthe solvent in the filtrate was distilled off under reduced pressure
  9. customThe residue was recrystallized from water-
  10. additioncontaining methanol

出典と根拠

ORDレコード
ord-ccbe35180d5349e08245fb39f2fbce2d
出典データセット
uspto-grants-1995_02
特許番号
US05387600

関連ノート

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