反应详情

To a solution of methyl 2-(2-chloro-4-fluorophenyl)-3-(oxiran-2-yl)propanoate (4.56 g, 17.6 mmol) in 2-propanol (20 mL) was added tert-butyl carbazate (2.3 g, 17.6 mmol) and the reaction heated to reflux for 16 hours. The reaction was then concentrated to dryness, redissolved in toluene (20 mL) and 1,5,7-triazobicylo(4.4.0)dec-5-ene (0.6 g, 4.4 mmol) was added and the mixture heated to reflux for 3 hours. The reaction was then diluted with ethylacetate, washed with 1 N HCl, dried with sodium sulfate and the solvent was evaporated in vacuo. The residue was recystallised from hot ethyl acetate to afford the title compound was obtained as a colourless solid (1.7 g, 26%). The mother liquor contained the trans isomer.

1. temperaturethe reaction heated
2. temperatureto reflux for 16 hours
3. concentrationThe reaction was then concentrated to dryness
4. dissolutionredissolved in toluene (20 mL)
5. temperaturethe mixture heated
6. temperatureto reflux for 3 hours
7. washwashed with 1 N HCl
8. dry with materialdried with sodium sulfate
9. customthe solvent was evaporated in vacuo