Formic Acid → HCID 57481674, compound

88% Formic acid (90 ml) and 30% hydrogen peroxide (3.17 ml) were added to 4-methoxy-1-cyclopentene thus obtained, and the mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, and a 35% aqueous solution of sodium hydroxide was added to the residue to alkalify the reaction mixture, followed by stirring at 50° C. for 10 minutes. The reaction mixture was cooled to room temperature and extracted with ethyl acetate to dry the organic layer over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography on silica gel (methanol:methylene chloride=1:19) to obtain the title compound (1.21 g).

1. customthus obtained
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additiona 35% aqueous solution of sodium hydroxide was added to the residue
4. stirringby stirring at 50° C. for 10 minutes
5. temperatureThe reaction mixture was cooled to room temperature
6. extractionextracted with ethyl acetate
7. dry with materialto dry the organic layer over anhydrous magnesium sulfate
8. distillationThe solvent was distilled off
9. customthe residue was purified by column chromatography on silica gel (methanol:methylene chloride=1:19)

ORD record

ord-2cdb64fcb5b046b9a141766f958851f6

Source dataset

uspto-grants-2008_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07342014B2