反应详情

温度

50 °C

3,3-Dimethylbutanal (0.7 mL, 5.4 mmol), tert-butyl 3-(aminomethyl)azetidine-1-carboxylate (Astatech™, 1.0 g, 5.4 mmol) were mixed with 2 g of 4 Å molecular sieves in 5 mL of dry acetonitrile at room temperature for 20 hours. The reaction was filtered through Celite, washed with 5 mL of acetonitrile and the filtrate used without further purification. Potassium thiocyanate (0.7 g, 7.1 mmol) was added and the mixture heated to 50° C. for 10 minutes. Iodine (1.4 g, 5.4 mmol) was added and the reaction mixture was continued to stir at 50° C. for 6 hours. The reaction mixture was cooled to room temperature, 10 mL of acetonitrile was added, followed byt 10 mL of 20% Na2S2O5. The phases were separated and the organic phase was dried with Na2SO4, filtered, and the solvent removed to provide the title compound. LC/MS m/z 326.3 (M+H)+. The product was used without further purification.

1. filtrationThe reaction was filtered through Celite
2. washwashed with 5 mL of acetonitrile
3. customthe filtrate used without further purification
4. temperatureThe reaction mixture was cooled to room temperature
5. customThe phases were separated
6. dry with materialthe organic phase was dried with Na2SO4
7. filtrationfiltered
8. customthe solvent removed