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
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
- customThe autoclave was closed
- custompurged with nitrogen
- customwas carried out for a total of 4 hours
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered through Celite®
- filtrationfilter aid
- washthe autoclave was rinsed with 50 g of isopropanol
- washthe filter cake was washed with 150 g of isopropanol
- distillationThe solvent was distilled from the combined filtrates and washings
- 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…