Acetonitrile → HCID 23158308, compound

310 mg of [hydroxy (p-nitrobenzenesulfonyloxy]iodo]benzene was added at room temperature to 20 ml solution of acetonitrile with 130 mg of 5-bromo-1-indanone, and the mixture was heated under reflux for 3 hours. The reaction solution was cooled down to room temperature, the solvents were distilled outunder reduced pressure. The obtained residues were dissolved in 20 ml of ethanol, and refluxed all night. The reaction solution was cooled down to room temperature, the solvents were distilled outunder reduced pressure, dissolved in ethyl acetate, washed with water and saturated saline solution, and dried with anhydrous sodium sulfate. The residues obtained by distilling out the solvents under reduced pressure were purified by silicagel column chromatography (hexane:ethyl acetate=95:5) to obtain 84 mg of the above compound as a white solid.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3 hours
3. distillationthe solvents were distilled outunder reduced pressure
4. dissolutionThe obtained residues were dissolved in 20 ml of ethanol
5. temperaturerefluxed all night
6. temperatureThe reaction solution was cooled down to room temperature
7. distillationthe solvents were distilled outunder reduced pressure
8. dissolutiondissolved in ethyl acetate
9. washwashed with water and saturated saline solution
10. dry with materialdried with anhydrous sodium sulfate
11. customThe residues obtained
12. distillationby distilling out the solvents under reduced pressure
13. customwere purified by silicagel column chromatography (hexane:ethyl acetate=95:5)

ORD record

ord-6233cd6d7626445eb344e377d2ca1deb

Source dataset

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07902369B2