반응 #76342

ord-05650c13c5504aa0a04f2489809bbca1

반응 방정식

NCc1cccc(OC(F)(F)F)c1
3-Trifluoromethoxybenzenemethanamine
FC(F)(F)C1CO1
1,1,1-trifluoro-2,3-epoxypropane
CC(O)(NCc1cccc(OC(F)(F)F)c1)C(F)(F)F
[[3-(trifluoromethoxy)-phenyl]methyl]amino-1,1,1-trifluoro-2-propanol

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

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) 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06699898B2uspto-grants-2004_03