Triethylamine → HCID 86685814, compound

Under a nitrogen atmosphere, 50 mL of dehydrated THF, 5.56 g (55.0 mmol) of triethylamine and 305 mg (2.5 mmol) of dimethylaminopyridine were added to 7.20 g (50.0 mmol) of 3,3,3-trifluorolactic acid at a room temperature. Thereafter, 5.75 g (55.0 mmol) of methacrylic acid chloride was added dropwise over 10 min, and then the mixture was stirred for 2 hrs. After disappearance of the raw material was confirmed by TLC, an aqueous sodium bicarbonate solution was added to stop the reaction. Thereafter, ethyl acetate was added to the reaction liquid and extraction was carried out three times. The organic layer thus obtained was washed with water, saturated brine each once, and dried by adding anhydrous sodium sulfate. Thereafter, the solvent was distilled off under a reduced pressure, and the resulting product was purified by column chromatography to give 3.71 g of 3,3,3-trifluoro-2-(methacryloyloxy)propionic acid represented by the following formula in the form of pale yellow oil (yield: 35%).

1. customthe reaction
2. customThe organic layer thus obtained
3. washwas washed with water, saturated brine each once, and
4. customdried
5. additionby adding anhydrous sodium sulfate
6. distillationThereafter, the solvent was distilled off under a reduced pressure
7. customthe resulting product was purified by column chromatography

ORD record

ord-403ae7d9acdf4913872c6a09931e24bd

Source dataset

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09261780B2