Methanol → 1,3-Diisobutyryloxyacetone

A 100 ml reaction vessel was charged with 4.18 g of dihydroxyacetone (monomer), 11.2 ml of pyridine and 10 mg of 4-dimethylaminopyridine and the mixture was stirred at room temperature. Thereto was added dropwise 16.7 ml of isobutyric anhydride over 30 minutes. After the dropping, the resulting liquid was further stirred for 1 hour and then 1 ml of methanol was added thereto and the resulting liquid was further stirred for 1 hour. To the reaction mixture was added ethyl acetate and the organic layer was separated. The organic layer was washed with water and further washed with saturated aqueous solution with sodium bicarbonate and 1N HCl. Then, the solvent was removed under reduced pressure. The residue was distilled under reduced pressure to give 7.47 g of the desired compound.

1. customA 100 ml reaction vessel
2. stirringAfter the dropping, the resulting liquid was further stirred for 1 hour
3. stirringthe resulting liquid was further stirred for 1 hour
4. customthe organic layer was separated
5. washThe organic layer was washed with water
6. washfurther washed with saturated aqueous solution with sodium bicarbonate and 1N HCl
7. customThen, the solvent was removed under reduced pressure
8. distillationThe residue was distilled under reduced pressure

ORD 기록

ord-a997e571454d4d2ca8243fa3c1bb3cc0

출처 데이터셋

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05840553