Potassium Carbonate → HCID 10430232, 화합물

Acetonitrile was added to a mixture of Compound 5A (about 1.0 mole), anhydrous potassium carbonate (about 1.5 moles) and tetrabutylammonium hydrogen sulfate (about 0.05 mole). 2-bromoethyl acetate (about 1.5 moles) was added in three separate portions (0.72 mole in the beginning, another 0.45 mole after about 2 hours of reaction, and then the remaining 0.33 mole after about another 1 hour of reaction) during the course of the reaction at about 80–85° C. The total reaction time was about 7 hours. The reaction mixture was cooled to about room temperature and filtered. The filtrate was concentrated. Aqueous isopropanol was added to crystallize the product. The product was filtered, washed with aqueous isopropanol, and dried to provide Compound 6A in about a 75–80% yield.

1. customseparate portions (0.72 mole in the beginning
2. customanother 0.45 mole after about 2 hours of reaction
3. customthe remaining 0.33 mole after about another 1 hour of reaction)
4. customduring the course of the reaction at about 80–85° C
5. temperatureThe reaction mixture was cooled to about room temperature
6. filtrationfiltered
7. concentrationThe filtrate was concentrated
8. additionAqueous isopropanol was added
9. customto crystallize the product
10. filtrationThe product was filtered
11. washwashed with aqueous isopropanol
12. customdried

ORD 기록

ord-417447cdb51a438bb0b0932df74ca360

출처 데이터셋

uspto-grants-2006_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07074923B2