Pyridine → Benzophenone oxime

HRID 273668

반응식

HRID 273668 반응식
[C:1]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:16][OH:17].N1C=CC=CC=1>C(O)C>[C:1](=[N:16][OH:17])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 3102BenzophenoneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 11324Benzophenone oxime수율 73%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of benzophenone (10.0 g), hydroxylamine hydrochloride (10.0 g), pyridine (50 ml), and absolute ethanol (50 ml) was pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa). The effluent was cooled and the solvent removed by rotary evaporation, and the residue stirred with cold water (50 ml). The crued oxime was filtered off and recrystallised from ethanol to afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5 for a batchwise preparation by microwave heating.

후처리

  1. customwas pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa)
  2. temperatureThe effluent was cooled
  3. customthe solvent removed by rotary evaporation
  4. filtrationThe crued oxime was filtered off
  5. customrecrystallised from ethanol
  6. customto afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5
  7. customfor a batchwise preparation by microwave
  8. temperatureheating

출처 및 근거

ORD 기록
ord-ac558e05036749a489f53ea207276d67
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387397

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