反应详情

温度

-30 °C

Nitrosonium tetrafluoroborate (2.415 g, 20.67 mmol) was added in several portions to a cooled (−30° C.) solution of 1,1-dimethylethyl cyclopropylcarbamate (2.5 g, 15.90 mmol) in anhydrous Pyridine (4 mL) and Acetonitrile (40 mL). The solution was stirred at −30° C. for 30 minutes then at 0° C. for 2 hours. Ice water and EtOAc were added. The organic phase was separated and washed with 1N HCl, 1N NaHCO3, brine, dried over MgSO4, filtered and concentrated in vacuo. The product was collected as 2.66 g. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 0.37-0.79 (m, 4 H), 1.64 (s, 9 H), 2.18-2.41 (m, 1 H).

1. waitat 0° C. for 2 hours
2. customThe organic phase was separated
3. washwashed with 1N HCl, 1N NaHCO3, brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe product was collected as 2.66 g