반응 #10415

반응 방정식

2-cyclopropylamino-4,5-difluorobenzoic acid

dichloromethane

methanol

(trimethylsilyl)diazomethane

→

title compound

2-cyclopropylamino-4,5-difluorobenzoic acid methyl ester

용매

formic acid

Water

반응 조건

후처리

1. 1
   추출the solution is extracted with dichloromethane
2. 2
   건조dried over MgSO4
3. 3
   여과filtered
4. 4
   기타the solvent removed under reduced pressure
5. 5
   기타The residue is purified by silica gel column chromatography

실험 절차

To a solution of 2-cyclopropylamino-4,5-difluorobenzoic acid (Example 5a) (6.0 g, 28.1 mmol), dichloromethane (100 mL), and methanol (20 mL) is added (trimethylsilyl)diazomethane (2.9 M solution in hexane) dropwise until the evolution of gas stops. The solution is stirred at room temperature for 0.5 hour and 88% formic acid is added dropwise until the evolution of gas again stops. Water is added, and the solution is extracted with dichloromethane, dried over MgSO4, filtered, and the solvent removed under reduced pressure. The residue is purified by silica gel column chromatography using hexane/EtOAc (9:1) as the eluent to afford a 5.4 g of the title compound as a clear oil. MS CI: m/z 228 (MH+).

출처