反应详情

温度

80 °C

Under a nitrogen atmosphere, methyl (3S,4R)-4-(4-chlorophenyl)-2-oxopyrrolidine-3-carboxylate (3.80 g, 15.0 mmol) was suspended in 1,2-dichlorobenzene (25 ml), and the suspension was poured into 6 mol/L hydrochloric acid (15.2 g). The mixture was reacted at 105° C. for 9 hours, then, cooled to 80° C. and the organic layer was separated by a liquid-separation operation. The aqueous layer was washed with 1,2-dichlorobenzene (11 ml), then, neutralized with a 20% sodium hydroxide aqueous solution to adjust pH to 7. The mixture was cooled to 15° C. and thermally insulated for 1 hour, then, the crystallized crystal was filtrated, and dried under reduces pressure, to obtain a title compound (2.69 g, 12.6 mmol)(yield: 84%). The optical purity of the resultant title compound was measured by HPLC to find a value of 99.9% ee or more (conditions are shown below).

1. customThe mixture was reacted at 105° C. for 9 hours
2. customthe organic layer was separated by a liquid-separation operation
3. washThe aqueous layer was washed with 1,2-dichlorobenzene (11 ml)
4. temperatureThe mixture was cooled to 15° C.
5. filtrationthe crystallized crystal was filtrated
6. customdried