반응 #84900

반응 방정식

methyl 4-bromo-2,6-difluorobenzoate

tert-butyl carbamate

Xantphos

caesium carbonate

→

Methyl 4-[(tert-butoxycarbonyl)amino]-2,6-difluorobenzoate

용매

1,4-dioxane

반응 조건

후처리

1. 1
   여과After filtration through kieselguhr
2. 2
   농축the filtrate was concentrated under reduced pressure
3. 3
   기타The crude product was purified by normal phase chromatography (mobile phase: dichloromethane/methanol 10-50% mixtures)

실험 절차

Under argon, a microwave vessel was charged with 54 mg (0.22 mmol) of methyl 4-bromo-2,6-difluorobenzoate, 118 mg (1.01 mmol, 4.7 eq.) of tert-butyl carbamate, 4.6 mg (0.02 mmol, 0.1 eq.) of palladium(II) acetate, 15 mg (0.026 mmol, 0.13 eq.) of Xantphos, 137 mg (0.42 mmol, 2 eq.) of caesium carbonate and 2 ml of 1,4-dioxane. A stream of argon was passed through the suspension for 2 min. The reaction mixture was heated in the microwave at 140° C. for 20 min. After filtration through kieselguhr, the filtrate was concentrated under reduced pressure. The crude product was purified by normal phase chromatography (mobile phase: dichloromethane/methanol 10-50% mixtures). Yield: 37 mg (60% of theory)

출처