2,6-Difluorobenzaldehyde → 2,6-Difluorobenzyl alcohol

HRID 365975

반응식

HRID 365975 반응식
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[CH:4]=[O:5]>[Pd]>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[CH2:4][OH:5]

참가 물질

3

반응 조건

온도
80 °C

실험 절차

332 g of 2,6-difluorobenzaldehyde were placed under nitrogen in a 0.7 1 autoclave and admixed with 6.4 g of 5% strength by weight palladium-on-carbon (catalyst from Heraeus type K-0227, containing 50% by weight of water). The autoclave was closed and purged with nitrogen. 50 bar of hydrogen were then injected and the contents of the autoclave were heated to 80° C. Hydrogenation was carried out for a total of 4 hours while stirring. After cooling and venting, the reaction mixture was filtered through Celite® filter aid, the autoclave was rinsed with 50 g of isopropanol and the filter cake was washed with 150 g of isopropanol. The solvent was distilled from the combined filtrates and washings and the crude product mixture was subsequently distilled off. 288 g of 2,6-difluorobenzyl alcohol were obtained (90% of theory).

후처리

  1. customThe autoclave was closed
  2. custompurged with nitrogen
  3. customwas carried out for a total of 4 hours
  4. temperatureAfter cooling
  5. filtrationthe reaction mixture was filtered through Celite®
  6. filtrationfilter aid
  7. washthe autoclave was rinsed with 50 g of isopropanol
  8. washthe filter cake was washed with 150 g of isopropanol
  9. distillationThe solvent was distilled from the combined filtrates and washings
  10. distillationthe crude product mixture was subsequently distilled off

출처 및 근거

ORD 기록
ord-f62e87a8e87c46dba8f0cccb66a62e20
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127581

연결된 노트

불러오는 중…