3-Bromo-1,1,1-trifluoro-2-propanone → 2-Propanone,3-bromo-1,1,1-trifluoro-, oxime

To a solution of 2.5 g of 1-bromo-3,3,3-trifluoropropan-2-one in 15 mL of chloroform (passed through a pad of basic alumina) was added a solution of hydroxylamine hydrochloride in 2.5 mL of water and the mixture heated to reflux. After 25 hours, the reaction mixture was cooled and 15 mL of H2O was added. The layers were separated and the aqueous layer was washed with 3×15 mL dichloromethane. The combined organic extracts were dried over magnesium sulfate, filtered and concentrated in vacuo. Note: As the product is a volatile liquid, excessive application of the vacuum to remove the co-solvent reduced the yield of the product. it's the product was used without further purification.

1. temperaturethe mixture heated to reflux
2. temperaturethe reaction mixture was cooled
3. customThe layers were separated
4. washthe aqueous layer was washed with 3×15 mL dichloromethane
5. dry with materialThe combined organic extracts were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto remove the co-solvent
9. customit's the product was used without further purification

ORDレコード

ord-348e3198a34444be969041a504e9902d

出典データセット

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08053442B2