Hydrochloric Acid → 2,4-Pentanedione, 3-(2-nitrobenzoyl)-

Magnesium ethoxide was generated by refluxing ethanol (50 mL) with 1.2 g (50 mmol) Magnesium turnings for 3 days. The ethanol was removed under reduced 10 pressure, and 50 mL of toluene was added, followed by dropwise addition of 5 g (50 mmol) of 2,5-pentanedione. The reaction mixture was stirred at room temperature for two hours and then at 70° C. for one hour, and then cooled to −10° C. A solution of 9.27 g (50 mmol) of 2-nitrobenzoyl chloride in 20 mL of toluene was added dropwise, and the solution was stirred at ambient temperature for 18 hours. The reaction mixture was 15 poured into a mixture of ice and 1N HCl, and the resulting solution was extracted with ethyl acetate. The organic layert was washed with brine, dried (MgSO4) filtered and concentrated to dryness under reduced pressure to afford 12.23 g of 3-(2-nitro-benzoyl)-pentane-2,4-dione

1. customThe ethanol was removed
2. additionwas added
3. waitat 70° C. for one hour
4. temperaturecooled to −10° C
5. stirringthe solution was stirred at ambient temperature for 18 hours
6. extractionthe resulting solution was extracted with ethyl acetate
7. washThe organic layert was washed with brine
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated to dryness under reduced pressure

ORDレコード

ord-be7c507f3f6445fc9c62e91db301e43b

出典データセット

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07776872B2