反应详情

温度

80 °C

An optically-active compound of [benzyl-(2-chloro-1-methylethyl)-amino]acetic acid tert-butyl ester (172.9 g) was dissolved in N,N-dimethylformamide (520 ml), and stirred at 80° C. for 140 minutes. The reaction mixture was cooled to 0° C. Then, thereto was added water (1200 ml), and the mixture was extracted with n-hexane/ethyl acetate (2/1, 1000 ml). The organic layer was sequentially washed with water (700 ml) and saturated aqueous sodium chloride solution (400 ml), and the separated aqueous layer was extracted with n-hexane/ethyl acetate (2/1, 600 ml) again. The combined organic layer was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=50/1 to 40/1) to give the titled compound (127.0 g).

1. temperatureThe reaction mixture was cooled to 0° C
2. extractionthe mixture was extracted with n-hexane/ethyl acetate (2/1, 1000 ml)
3. washThe organic layer was sequentially washed with water (700 ml) and saturated aqueous sodium chloride solution (400 ml)
4. extractionthe separated aqueous layer was extracted with n-hexane/ethyl acetate (2/1, 600 ml) again
5. concentrationThe combined organic layer was concentrated under reduced pressure
6. customthe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=50/1 to 40/1)