반응 #76342
ord-05650c13c5504aa0a04f2489809bbca1
반응 방정식
3-Trifluoromethoxybenzenemethanamine
1,1,1-trifluoro-2,3-epoxypropane
→
[[3-(trifluoromethoxy)-phenyl]methyl]amino-1,1,1-trifluoro-2-propanol
반응 조건
온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The mixture was cooled to room temperature
- 2기타the resulting solid was recrystallized from hot hexanes
- 3기타The white solid was isolated by vacuum filtration
- 4세척washed with cold hexanes
실험 절차
Ex-632A) 3-Trifluoromethoxybenzenemethanamine (1.15 g, 6 mmol) and 1,1,1-trifluoro-2,3-epoxypropane (0.67 g, 6 mmol) were combined and stirred at 80° C. for 1.5 h. The mixture was cooled to room temperature, and the resulting solid was recrystallized from hot hexanes. The white solid was isolated by vacuum filtration and washed with cold hexanes to give 0.67 g (37%) of pure 3-[[[3-(trifluoromethoxy)-phenyl]methyl]amino-1,1,1-trifluoro-2-propanol. 1H NMR (CDCl3) δ7.37 (t, 1H), 7.24 (d, 1H), 7.15 (m, 2H), 3.99 (m, 1H), 3.85 (d, 2H), 2.98 (dd, 1H), 2.88 (dd, 1H), 2.79 (s, 1H). 19F NMR (CDCl3) δ−58.19 (s, 3F), −78.88 (s, 3F). HRMS calcd. for C11H11F6NO2: 304.0772 [M+H]+, found: 304.0794.