Carbamic acid, ethyl ester → Ethyl (2-methylacryloyl)carbamate

Temperature

60 °C

To the solution of 8.9 g of ethyl carbamate in 100 g of THF, 11.2 g of potassium t-butoxide was mixed and the reaction mixture was stirred for 1 hour at 60° C. The resulting slurry was added dropwise to the solution of 5.43 g of methacryloyl acid chloride in 50 g of THF heated at 60° C. in 2 hours. After removing THF by vacuum evaporation, the residue was extracted with 1000 ml of water and 500 ml of ethyl acetate. The organic phase was concentrated in vacuo and the residue was subjected to column chromatography for purification, thereby isolating 1.0 g of ethyl methacryloylcarbamate.

1. temperatureheated at 60° C. in 2 hours
2. customAfter removing THF
3. customby vacuum evaporation
4. extractionthe residue was extracted with 1000 ml of water and 500 ml of ethyl acetate
5. concentrationThe organic phase was concentrated in vacuo
6. customthe residue was subjected to column chromatography for purification

ORD record

ord-cac834d7774748a98d9a69a2e72de78f

Source dataset

uspto-grants-1993_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05187306