反应详情

温度

5 °C

N-tert-Butoxycarbonyl-D-leucine monohydrate (25.00 g) was dissolved in tetrahydrofuran (224 mL), and triethylamine (20.30 g) and isobutyl chlorocarbonate (13.06 g) were sequentially added thereto at 5° C. or lower under cooling on ice. To the mixture was added 3-amino-8-(2-oxopyrrolidin-1-yl)-1-(thiophen-3-ylmethyl)-3,4-dihydroquinolin-2(1H)-one D-(−)-tartrate (44.80 g) in an aqueous sodium hydroxide solution (a mixture of 25% aqueous sodium hydroxide solution (14.58 g) and water (89.6 g)) at 5° C. or lower. The mixture was stirred for 10 minutes under cooling on ice, and then the temperature was raised to room temperature. Saturated aqueous sodium chloride solution (44.8 g) was added to the reaction mixture to partition the mixture, and the aqueous layer was further extracted with tetrahydrofuran (224 mL). The organic layers were combined, and the combined organic layer was concentrated to half volume, whereby a solution of the title compound in tetrahydrofuran was yielded.

1. temperatureunder cooling on ice
2. temperaturethe temperature was raised to room temperature
3. customto partition the mixture
4. extractionthe aqueous layer was further extracted with tetrahydrofuran (224 mL)
5. concentrationthe combined organic layer was concentrated to half volume, whereby a solution of the title compound in tetrahydrofuran
6. customwas yielded