Dichloromethane → t-Butyl isobutyrylacetate

In a mixture of 85 ml of dichloromethane and 40 ml of pyridine was dissolved 33.8 g of meldrum's acid. Under cooling with ice, 25.0 g of isobutyl chloride was added dropwise to the solution, followed by stirring under room temperature for 1 hour. The solvent was removed under reduced pressure and to the residue was added water. The mixture was extracted with ethyl acetate. The extract was washed with 1N hydrochloric acid and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the residue was dissolved in 100 ml of tert-butanol, followed by reflux under heating for 4 hours. The solvent was removed under reduced pressure. The residue was subjected to distillation under reduced pressure to yield 32.5 g of the oily titled compound.

1. additionwas added dropwise to the solution
2. customThe solvent was removed under reduced pressure and to the residue
3. additionwas added water
4. extractionThe mixture was extracted with ethyl acetate
5. washThe extract was washed with 1N hydrochloric acid
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was removed under reduced pressure
8. dissolutionthe residue was dissolved in 100 ml of tert-butanol
9. temperatureby reflux
10. temperatureunder heating for 4 hours
11. customThe solvent was removed under reduced pressure
12. distillationThe residue was subjected to distillation under reduced pressure

ORDレコード

ord-271293b68ebc45b4acc42dbcd5d0b96f

出典データセット

uspto-grants-1997_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05599813