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

HRID 261507노트

반응식

HRID 261507 반응식
[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

참가 물질

4

반응물 2

HCID 6407ChloralHCID 11955Benzoylhydrazine

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b39336166e5b4ab5b399ac435939e4a4
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166129

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