Chloral → Benzoic acid, 2-(2,2,2-trichloroethylidene)hydrazide

HRID 261507ノート

反応式

HRID 261507 の反応式
[C:1]([NH:9][NH2:10])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O=[CH:12][C:13]([Cl:16])([Cl:15])[Cl:14]>C1C=CC=CC=1>[C:1]([NH:9][N:10]=[CH:12][C:13]([Cl:16])([Cl:15])[Cl:14])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 6407ChloralHCID 11955Benzoylhydrazine

生成物 1

HCID 53650662Benzoic acid, 2-(2,2,2-trichloroethylidene)hydrazide

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

10 g (0.073 mol) of benzoylhydrazine were suspended in benzene, 200 ml, and 18.3 g (0.124 mol) of chloral were added dropwise to the suspension which was then refluxed under agitation for 3 hours. Upon cooling, the sedimented crystals were collected by filtration and washed well with benzene. In this way, white brown crystals, 19 g, were obtained substantially quantatively. m.p. 188°-189° C. (decomposed). When recrystallized from acetone, the Compound No. 1, m.p. 194°-195° (decomposed), was obtained in white needles. Yield: 15.4 g (81% of the theoretical).

後処理

  1. temperaturewas then refluxed under agitation for 3 hours
  2. temperatureUpon cooling
  3. filtrationthe sedimented crystals were collected by filtration
  4. washwashed well with benzene
  5. customIn this way, white brown crystals, 19 g, were obtained substantially quantatively
  6. customWhen recrystallized from acetone
  7. custom1, m.p. 194°-195° (decomposed), was obtained in white needles

出典と根拠

ORDレコード
ord-b39336166e5b4ab5b399ac435939e4a4
出典データセット
uspto-grants-1979_08
特許番号
US04166129

反応ノート

読み込み中…