4H-1-Benzopyran-2-carboxylic acid, 4-oxo-, methyl ester → HCID 12536095, compound

500 mg of methyl 4-oxo-4H-chromene-2-carboxylate were dissolved in 25 ml of anhydrous methanol at room temperature, and NaBH4 was thereafter added to the solution slowly, until the starting material was no longer detected by TLC (about 300 mg). The solvent was then evaporated and a mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water was added to the resulting residue. The pH of the mixture was maintained between 5 and 9, so as to prevent decomposition of chromone. The aqueous solution was washed with chloroform (3×50 ml) and the combined organic extracts were dried over Na2SO4. The solvent was evaporated to give 2-(hydroxymethyl)-4H-chromen-4-one which was used without future purification.

1. customThe solvent was then evaporated
2. additiona mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water
3. additionwas added to the resulting residue
4. temperatureThe pH of the mixture was maintained between 5 and 9
5. washThe aqueous solution was washed with chloroform (3×50 ml)
6. dry with materialthe combined organic extracts were dried over Na2SO4
7. customThe solvent was evaporated

ORD record

ord-cfc367471d9e424f9b8be84b6d252a78

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09034872B2