反応 #1565073

反応方程式

product

N-(1-(3-(4-chlorophenyl)-1-cyanopent-1-yn-3-yl)-1H-indol-4-yl)-N-((2-(trimethylsilyl)ethoxy)methyl)methanesulfonamide

HCl

→

title compound

N-(1-(3-(4-chlorophenyl)-1-cyanopent-1-yn-3-yl)-1H-indol-4-yl)methanesulfonamide

溶媒

EtOH

反応条件

後処理

1. 1
   その他The volatile was removed under reduced pressure
2. 2
   その他the residue was purified by Combiflash (Mobile phase

実験手順

To a solution of the product from step D (15 mg, 0.028 mmol, enantiomer A) in EtOH (2 mL) was added 2N HCl (0.5 mL). The mixture was stirred at 50° C. overnight. The volatile was removed under reduced pressure and the residue was purified by Combiflash (Mobile phase: MeOH/H2O (0.08% of NH4HCO3) to obtain the title compound. LC/MS m/z=412.1 [M+H]+. 1H NMR (400 MHz, CDC13) δ: 7.53 (d, J=3.6 Hz, 1H), 7.33 (d, J=8.8 Hz, 2H), 7.17 (d, J=8.0 Hz, 1H), 7.12 (d, J=8.4 Hz, 2H), 7.01 (t, J=8.0 Hz, 1H), 6.73 (d, J=8.4 Hz, 1H), 6.70 (d, J=3.6 Hz, 1H), 6.62 (br, 1H), 3.04 (s, 3H), 2.80-2.76 (m, 1H), 2.52-2.48 (m, 1H), 1.05 (t, J=7.2 Hz, 3H).

出典