反应详情

温度

15 °C

Ethyl 2-(tert-butoxycarbonylamino)-2-cyanoacetate (1.20 g, 526 mmol) prepared in the same manner as Reference Example 1, acetone (2.3 ml), powdered potassium carbonate (872 mg, 6.31 mmol) and potassium iodide (175 mg, 1.05 mmol) were mixed, a solution of menthyl chloroacetate (1.22 g, 5.26 mmol) dissolved in acetone (1.1 ml) was added dropwise thereto at 10-20° C., and the mixture was stirred at the same temperature overnight. Insoluble materials were removed by filtration, the filtrate was concentrated in vacuo and toluene was added to the residue. The organic layer was washed with water and concentrated in vacuo to give ethyl 2-(tert-butoxycarbonylamino)-2-cyano-3-[(−)menthyloxycarbonyl]propionate (1.10 g, yield 49.3%) as a yellow oil.

1. additionwere mixed
2. additionwas added dropwise
3. customInsoluble materials were removed by filtration
4. concentrationthe filtrate was concentrated in vacuo and toluene
5. additionwas added to the residue
6. washThe organic layer was washed with water
7. concentrationconcentrated in vacuo