반응 #78775

반응 방정식

3-Trifluoromethoxybenzenemethanamine

1,1,1-trifluoro-2,3-epoxypropane

→

3-[[[3-(trifluoromethoxy)-phenyl]methyl]amino]-1,1,1-trifluoro-2-propanol

수율 37.0%

반응 조건

후처리

1. 1
   온도The mixture was cooled to room temperature
2. 2
   기타the resulting solid was recrystallized from hot hexanes
3. 3
   기타The white solid was isolated by vacuum filtration
4. 4
   세척washed 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) δ 7.37 (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.

출처