反应详情

In a 25-mL glass flask with a dropping funnel, 5.0 g (82.2 mmol/4.0 eq) of 28% aqueous ammonia solution was added and stirred. Subsequently, 5.0 g (purity: 98%, 20.4 mmol) of methacrylic acid 1-chlorocarbonyl-1,1-difluoro-2-butyl ester was dropped into the glass flask. The resulting solution was stirred for 10 minutes at room temperature. The completion of the reaction was confirmed by 19F NMR. After that, the solution was separated into an organic layer and an aqueous layer with the addition of 5 mL of water and 5 mL of diisopropyl ether. The thus-obtained aqueous layer was concentrated under a reduced pressure. With this, 4.1 g of methacrylic acid 1-aminocarbonyl-1,1-difluoro-2-butyl ester was obtained as a white crystalline substance (yield: 86%, purity: 96%).

1. stirringThe resulting solution was stirred for 10 minutes at room temperature
2. customAfter that, the solution was separated into an organic layer
3. additionan aqueous layer with the addition of 5 mL of water and 5 mL of diisopropyl ether
4. concentrationThe thus-obtained aqueous layer was concentrated under a reduced pressure