Phenyl Isothiocyanate → HCID 21427813、化合物

HRID 437521ノート

反応式

HRID 437521 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])=[CH:4][CH:3]=1.[C:16]1([N:22]=[C:23]=[S:24])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C(O)C>[C:16]1([NH:22][C:23](=[S:24])[NH:1][C:2]2[CH:3]=[CH:4][C:5]([NH:8][NH:9][C:10](=[O:15])[C:11]([F:12])([F:13])[F:14])=[CH:6][CH:7]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

4

反応物 2

HCID 7673Phenyl IsothiocyanateHCID 11148694HCID 11148694、化合物

生成物 1

HCID 21427813HCID 21427813、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-(4-Aminophenyl)-1-trifluoroacetylhydrazine (2.0 g, 0.0091 mole) and phenyl isothiocyanate (1.2 g, 0.0091 mole) were mixed together in ethanol (25 ml) and the mixture was heated to reflux for 20 minutes. A white solid precipitated out of the mixture during the heating. The mixture was chilled in ice and the solid was filtered off, washed with ethanol, and dried. Spectral data on this material indicated that it was not the desired product. The filtrate from above was diluted with water and a second solid material formed. This material was filtered off, washed with water and dried to give a white crystalline powder. Yield 0.80 g (25%), m.p. 172°-174° C. Spectral evidence verified that this substance was the desired product.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 20 minutes
  3. customA white solid precipitated out of the mixture during the heating
  4. temperatureThe mixture was chilled in ice
  5. filtrationthe solid was filtered off
  6. washwashed with ethanol
  7. customdried
  8. additionThe filtrate from above was diluted with water
  9. customa second solid material formed
  10. filtrationThis material was filtered off
  11. washwashed with water
  12. customdried
  13. customto give a white crystalline powder

出典と根拠

ORDレコード
ord-d49c3926d8314431a026b677fc453b36
出典データセット
uspto-grants-1977_06
特許番号
US04031127

反応ノート

読み込み中…