반응 #1012270

반응 방정식

3-amino-4-fluorobenzoic acid

cesium carbonate

benzyl chloroformate

→

title compound

3-(benzyloxycarbonylamino)-4-fluorobenzoic acid

용매

tetrahydrofuran

water

반응 조건

후처리

1. 1
   농축was concentrated to about 200 mL
2. 2
   기타was partitioned between ethyl acetate and brine
3. 3
   여과The precipitated solid was collected by filtration
4. 4
   세척washed with ethyl acetate and water
5. 5
   기타dried

실험 절차

To a solution of 3-amino-4-fluorobenzoic acid (30 g, 193 mmol) in a mixture of tetrahydrofuran (300 mL) and water (300 mL) was added cesium carbonate (157 g, 483 mmol) and benzyl chloroformate (30.4 mL, 213 mmol). This mixture was stirred at ambient temperature for 16 hours, and was concentrated to about 200 mL. The residue was acidified with 2N HCl to a pH 3, and was partitioned between ethyl acetate and brine. The precipitated solid was collected by filtration, washed with ethyl acetate and water, and dried to provide the title compound. MS (DCI/NH3) m/z 290 (M+H)+.

출처