反应详情

温度

22.5 °C

In a 2 flask were charged 275 ml of methylene chloride, 550 ml of cyclohexane, 140 g of benzyl trichloroacetoimidate, and 75 g of methyl (S)-3-hydroxyheptanoate (compound (37), R1 =ethyl), and 6 ml of trifluoromethanesulfonic acid was added thereto over 5 minutes while maintaining at 20 to 25° C., followed by allowing the mixture to react at 35 to 40° C. for 5 hours. The by-produced salt was removed by filtration, and the filtrate was washed with a sodium hydrogencarbonate aqueous solution. The solvent was removed by distillation under reduced pressure, and the residue was distilled under reduced pressure to obtain 99.0 g (78.7%) of the titled compound (b.p.: 105-108° C./0.1 mmHg).

1. additionwas added
2. customto react at 35 to 40° C. for 5 hours
3. customThe by-produced salt was removed by filtration
4. washthe filtrate was washed with a sodium hydrogencarbonate aqueous solution
5. customThe solvent was removed by distillation under reduced pressure
6. distillationthe residue was distilled under reduced pressure