Diisopropylethylamine → 4-((3-ethylphenyl)(2-methyl-5-phenyl-2H-1,2,4-triazol-3-yl)methylamino)-3-fluorobenzonitrile

関与物質

反応条件

反応手順

Methansulfonic anhydride (77 mg, 0.44 mmol) was added to a solution of Intermediate 370.2 (81 mg, 0.28 mmol) and diisopropylethylamine (0.2 mL, 1.16 mmol) in CH2Cl2 (2.5 mL) at 0° C. The mixture was stirred for 1 h at 0° C. and then 4-amino-3-fluorobenzonitrile (136 mg, 1 mmol) was added. The mixture was stirred for 1 h at ambient temperature, diluted with CH2Cl2 (40 mL), washed with sat. NaHCO3 and brine, dried (Na2SO4) and concentrated. Purification by flash chromatography (EtOAc, hexanes) afforded 65 mg of Intermediate 382.1. 1H NMR (400 MHz, CDCl3) δ ppm 1.11 (t, J=7.58 Hz, 3H) 2.54 (q, J=7.58 Hz, 2H) 3.69 (s, 3 H) 5.60 (d, J=5.87 Hz, 1H) 6.10-6.16 (m, J=1.96 Hz, 1H) 7.06-7.24 (m, 6H) 7.27-7.39 (m, 3H) 7.99-8.04 (m, 2H).

情報源と証拠