Hydrochloric Acid → HCID 20220949, compound

To all of the compound obtained in step (a) above were added 39 g of sodium hydroxide and 120 ml of propylene glycol, and the mixture was stirred at room temperature for 10 minutes. The liquid reaction mixture was made acidic by addition of 6N hydrochloric acid and was extracted with benzene. The extract was washed with water and dried, and the solvent was removed by distillation. The residue was dissolved in 120 ml of pyridine and 0.6 g of copper powder was added to the solution. The mixture was refluxed for 2 hours, and the copper powder was removed by filtration and the solvent was removed by distillation. The residue was dissolved in n-hexane, and the solution was washed with water and dried. The solvent was removed by distillation and the residue was purified by column chromatography using silica gel to obtain 45 g of the intended compound in the form of an oil.

1. customThe liquid reaction mixture
2. extractionwas extracted with benzene
3. washThe extract was washed with water
4. customdried
5. customthe solvent was removed by distillation
6. dissolutionThe residue was dissolved in 120 ml of pyridine
7. addition0.6 g of copper powder was added to the solution
8. temperatureThe mixture was refluxed for 2 hours
9. customthe copper powder was removed by filtration
10. customthe solvent was removed by distillation
11. dissolutionThe residue was dissolved in n-hexane
12. washthe solution was washed with water
13. customdried
14. customThe solvent was removed by distillation
15. customthe residue was purified by column chromatography

ORD record

ord-d2a6032cf9684fc297ded0ab4c76abe5

Source dataset

uspto-grants-1984_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04456603