Hydrochloric Acid → HCID 20827730, compound

Ethyl 2,4-dichlorophenylcarbamate (1.206 g) was dissolved in tetrahydrofuran (15 ml), and to the solution were added sodium hydride (206.0 mg) and 2-chloro-3,5-dinitrobenzotrifluoride (1.161 g). The reaction mixture was stirred at room temperature for 4 hours. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=5:1) to give the title compound (1.4490 g, 72%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe resultant residue was purified by silica gel column (75 g, hexane:ethyl acetate=5:1)

ORD record

ord-c12b8cda65d84a69b8114dab87462ef2

Source dataset

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06939887B2