Hydrochloric Acid → HCID 20220949, compound

To the entirety of the product obtained in the above (a) step, there were added 39 g. of sodium hydroxide and 120 ml. of propylene glycol, and the mixture was stirred at room temperature for 10 min. The reaction mixture was then made acidic by addition of 6N hydrochloric acid, and was then extracted with benzene. The extract was then washed with water and dried. The solvent was then removed by evaporation. The residue was dissolved in 120 ml. of pyridine, and the resulting solution was refluxed for 2 hours after addition of 0.6 g. of copper powder. Subsequently, the copper powder was removed by filtration and the solvent was removed by evaporation. The residue was dissolved in n-hexane, washed with water and dried. The solvent was then removed by evaporation, and the residue was purified by silica gel column chromatography to obtain 45 g. of the desired oily product.

1. additionwere added 39 g
2. extractionwas then extracted with benzene
3. washThe extract was then washed with water
4. customdried
5. customThe solvent was then removed by evaporation
6. dissolutionThe residue was dissolved in 120 ml
7. temperatureof pyridine, and the resulting solution was refluxed for 2 hours
8. additionafter addition of 0.6 g
9. customSubsequently, the copper powder was removed by filtration
10. customthe solvent was removed by evaporation
11. dissolutionThe residue was dissolved in n-hexane
12. washwashed with water
13. customdried
14. customThe solvent was then removed by evaporation
15. customthe residue was purified by silica gel column chromatography
16. customto obtain 45 g

ORD record

ord-23c73064b5c141e1a84a7101bb169097

Source dataset

uspto-grants-1984_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04481217