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

温度

80 °C

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).

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

ORDレコード

ord-f62e87a8e87c46dba8f0cccb66a62e20

出典データセット

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06127581