Sodium Hydroxide → Methyl 2,2-dimethyl-3-oxopropanoate

Temperature

0 °C

To a stirred solution of methyl 2,2-dimethyl-3-hydroxypropionate (1 g, 7.57 mmol) in DCM (50 ml) at 0° C. under nitrogen was added Dess-Martin periodinane (3.21 g, 7.57 mmol) in one portion and the reaction mixture was stirred at 0° C. for 1 h then rt for 45 min. The reaction mixture was cooled down to 0° C. and poured into 1N NaOH solution (30 mL) and extracted with DCM. The organic layer was collected, dried over anhydrous magnesium sulfate, filtered, and partially evaporated (at around 25° C.) under reduced pressure, to afford a solution of 567 that was stored in the freezer and used in the next step without any further purification.

1. waitrt for 45 min
2. temperatureThe reaction mixture was cooled down to 0° C.
3. extractionextracted with DCM
4. customThe organic layer was collected
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. custompartially evaporated (at around 25° C.) under reduced pressure

ORD record

ord-1647ba3a18664b8aa9bd0d711223afb1

Source dataset

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08906852B2