反应详情

N-(Hydroxymethyl)trifluoroacetamide (70 mmol; 10.0 g) was added to a mixture of 2-chlorobenzoic acid (70 mmol; 10.9 g) and conc. H2SO4 (120 mL). The mixture was stirred at rt overnight, poured into ice water and stirred for 2 h. The precipitate was collected by filtration, dried and recrystallised from toluene/butan-2-one (7:1) to give the subtitle compound. Yield: 9.6 g (49%). MS [M−H]−=280 (Cl isotope pattern), TLC: Rf=0.57 (RP-8, MeOH:5%-aq NaCl-solution 6:4).

1. stirringstirred for 2 h
2. filtrationThe precipitate was collected by filtration
3. customdried
4. customrecrystallised from toluene/butan-2-one (7:1)