反应详情

温度

0 °C

Treat a solution of 2-(1-(trifluoromethyl)cyclopropyl)acetonitrile (2.2 g, 14.7 mmol) in THF (60 mL), under N2, with BH3 (10 M in dimethyl sulfide, 3 mL, 30 mmol) and heat at 70° C. overnight. Cool the mixture to 0° C., treat dropwise with methanolic HCl, concentrate to dryness, dissolve in MeOH, re-concentrate and treat the residue with EtOAc. Collect the solids via filtration and dry to afford the title compound (1.1 g, 40% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.05 (s, 3H), 2.87 (t, J=8.4 Hz, 2H), 1.90-1.86 (m, 2H), 0.96-0.93 (m, 2H), 0.82-0.81 (m, 2H).

1. concentrationconcentrate to dryness
2. dissolutiondissolve in MeOH
3. concentrationre-concentrate
4. additiontreat the residue with EtOAc
5. customCollect the solids
6. filtrationvia filtration
7. customdry