Hydrochloric Acid → 8-(propan-2-yl)-3,4-dihydro-2H-1-benzopyran-4-one

온도

-20 °C

3-(2-Isopropylphenoxy)propionic acid (11) was dissolved in dichloromethane (30 mL), and to the mixture were added oxalyl chloride (2.1 g) and DMF (5 mL) under ice-cooling. The reaction mixture was stirred for 30 minutes and cooled at −20° C. To the reaction mixture was added aluminium chloride (4 g), and the reaction mixture was stirred at −20° C. for 2 h. To the reaction mixture was added 2N hydrochloric acid, and the reaction mixture was extracted with dicloromethane. The organic layer was washed with brine, dried over magnesium sulfate, and evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1) to obtain the compound (12) 2.3 g.

1. temperaturecooling
2. stirringthe reaction mixture was stirred at −20° C. for 2 h
3. extractionthe reaction mixture was extracted with dicloromethane
4. washThe organic layer was washed with brine
5. dry with materialdried over magnesium sulfate
6. customevaporated
7. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate=4:1)

ORD 기록

ord-e39558ed39c74c57b61429847866e967

출처 데이터셋

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07601746B2