反应详情

3,3-Dimethylbutanal (0.95 g, 9.1 mmol), 3-methylbut-2-en-1-amine hydrochloride (1.1 g, 9.1 mmol), and triethylamine (1.3 mL, 9.1 mmol) were mixed in 9 mL of dry MeCN with 2 g of 4 Å (8-12 mesh beads) molecular sieves and stirred for 20 hours at room temperature. The reaction was filtered through Celite and washed with 8 mL of MeCN. KSCN (1.2 g, 12.3 mmol) was added and the mixture warmed to 50° C. Iodine (2.3 g, 9.1 mmol) was added and the reaction stirred at 50° C. for 6 hours. 20% Na2S2O5 was added, stirred for 30 minutes and the organic layer separated, dried with Na2SO4 and the solvent removed. The resulting solid was used without further purification. LC/MS m/z 225.3 (M+H)+.

1. filtrationThe reaction was filtered through Celite
2. washwashed with 8 mL of MeCN
3. temperaturethe mixture warmed to 50° C
4. stirringthe reaction stirred at 50° C. for 6 hours
5. stirringstirred for 30 minutes
6. customthe organic layer separated
7. dry with materialdried with Na2SO4
8. customthe solvent removed
9. customThe resulting solid was used without further purification