Water → 3-Bromo-4-fluorobenzaldehyde

HRID 851284

반응식

HRID 851284 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[C:5]#N.[OH2:11]>[Ni].C(O)=O>[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH:5]=[O:11]

참가 물질

5

반응물 2

HCID 962WaterHCID 1235793-Bromo-4-fluorobenzonitrile

생성물 1

HCID 1736043-Bromo-4-fluorobenzaldehyde수율 85%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 284Formic Acid용매

실험 절차

17.0 g of a 50% strength alkaline suspension of Raney nickel were filtered under a nitrogen atmosphere and the material on the filter was washed until neutral. The Raney nickel obtained by this method was suspended in 150 ml of formic acid. 20.0 g (0.1 mole) of 3-bromo-4-fluoro-benzonitrile were added to this suspension. The mixture was heated at 80° to 90° C. for 3 to 5 hours and the reaction mixture was then cooled and poured into 300 ml of water. After filtering, the filtrate was twice extracted with, in each case, 200 ml of toluene. The toluene phase was dried over sodium sulphate and then concentrated. 17.2 g (85% of theory) of 3-bromo-4-fluoro-benzaldehyde with a boiling point of 63°-65° C./0.3 mm Hg were obtained.

후처리

  1. filtrationwere filtered under a nitrogen atmosphere
  2. washthe material on the filter was washed until neutral
  3. customThe Raney nickel obtained by this method
  4. temperatureThe mixture was heated at 80° to 90° C. for 3 to 5 hours
  5. temperaturethe reaction mixture was then cooled
  6. filtrationAfter filtering
  7. extractionthe filtrate was twice extracted with, in each case, 200 ml of toluene
  8. dry with materialThe toluene phase was dried over sodium sulphate
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a7d4e6788f22427e80515f37aff1301f
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04383949

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