HCID 86750616, compound → HCID 44329557, compound

A mixture of 0.50 g of 2-(3,4-epoxy-6-pentafluoroethyl-2,2-bisfluoromethyl-3,4-dihydro-2H-1-benzopyran-4-yl)pyridine N-oxide, 0.10 g of 10% palladium carbon and 15 ml of methanol was stirred at room temperature under hydrogen stream. The-reaction mixture was subjected to vacuum filtration to remove the catalyst and the mother liquor was distilled off. The resultant residue was dissolved in 10 ml of dioxane and 0.82 g of soda talc was added thereto. The mixture was refluxed with heating for 1 hour and subjected to vacuum filtration to remove insoluble materials. Water was added to the mother liquor and the mixture was extracted with methylene chloride. The organic layer was washed with water and dried. The solvent was distilled off and the resultant residue was purified using silica gel column chromatography (developing solution, MeOH:CH2Cl2 =1:99) to obtain 0.18 g of 2-(6-pentafluoroethyl-2,2-bisfluoromethyl-2H-1-benzopyran-4-yl)pyridine N-oxide.

1. customThe-reaction mixture
2. filtrationwas subjected to vacuum filtration
3. customto remove the catalyst
4. distillationthe mother liquor was distilled off
5. dissolutionThe resultant residue was dissolved in 10 ml of dioxane
6. addition0.82 g of soda talc was added
7. temperatureThe mixture was refluxed
8. temperaturewith heating for 1 hour
9. filtrationsubjected to vacuum filtration
10. customto remove insoluble materials
11. additionWater was added to the mother liquor
12. extractionthe mixture was extracted with methylene chloride
13. washThe organic layer was washed with water
14. customdried
15. distillationThe solvent was distilled off
16. customthe resultant residue was purified

ORD record

ord-5c113eccc55f4837bcf8491d0cb2ffa1

Source dataset

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05874446