Glycine ethyl ester, hydrochloride → N-(2,4-difluorophenyl)-N'-ethoxycarbonylmethylurea

Temperature

80 °C

Phenyl 2,4-difluorophenylcarbamate (5.0 g) and 4.2 g of glycine ethyl ester hydrochloride were dissolved in 30 ml of pyridine and the solution was heated at 80° C. for 14 hours. The reaction solution was concentrated under reduced pressure and to the residue were added 80 ml of ethyl acetate and 20 ml of water. The ethyl acetate layer was washed with 10 ml of an aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Hexane (50 ml) was added to the residue and the solid separated out was collected by filtration to give 4.58 g of N-(2,4-difluorophenyl)-N'-ethoxycarbonylmethylurea as a colorless powder.

1. concentrationThe reaction solution was concentrated under reduced pressure and to the residue
2. additionwere added 80 ml of ethyl acetate and 20 ml of water
3. washThe ethyl acetate layer was washed with 10 ml of an aqueous solution of sodium chloride
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. additionHexane (50 ml) was added to the residue
7. customthe solid separated out
8. filtrationwas collected by filtration

ORD record

ord-6b2e87eaf21f4ac686825e81b4605c5f

Source dataset

uspto-grants-1998_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05792780