2,6-Dimethyl-4-pyranone → Tetrahydro-2,6-dimethyl-4H-pyran-4-one

A solution of 2,6-dimethyl-γ-pyrone (17 g) in 300 mL of EtOH 95% was hydrogenated for 3 days under 70 psi. After filtration over celite, without extraction, the solvent was evaporated and replaced by CH2Cl2. The solution was then treated with 30 g of celite and 48.5 g of pyridinium chlorochromate. The suspension was stirred for 3 hr. and the reaction was diluted with 300 mL of Et2O and then filtered over a pad of celite. The filtrate was evaporated to dryness and the residual solution was then chromatographed using hexane/ether (1:1) to give the title compound.

1. filtrationAfter filtration over celite
2. extractionwithout extraction
3. customthe solvent was evaporated
4. additionThe solution was then treated with 30 g of celite and 48.5 g of pyridinium chlorochromate
5. additionand the reaction was diluted with 300 mL of Et2O
6. filtrationfiltered over a pad of celite
7. customThe filtrate was evaporated to dryness
8. customthe residual solution was then chromatographed

ORDレコード

ord-79679b8eaad24158bd56247af47c5bdb

出典データセット

uspto-grants-1993_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05227399