Pyridine → Benzophenone oxime

HRID 273668

反応式

HRID 273668 の反応式
[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

参加物

5

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ac558e05036749a489f53ea207276d67
出典データセット
uspto-grants-1995_02
特許番号
US05387397

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