反応 #10806

反応方程式

4-{3-[4-Methoxy-2-(2-morpholin-4-yl-ethoxy)-5-thiophen-2-yl-phenyl]-acryloyl}-benzenesulfonamide

HCl

→

title compound

収率 78.0%

4-{3E-[4-Methoxy-2-(2-morpholin-4-yl-ethoxy)-5-thiophen-2-yl-phenyl]-acryloyl}-benzenesulfonamide, hydrochloride

収率 78.0%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他The precipitate was collected
2. 2
   その他dried in vacuo

実験手順

Th 4-{3-[4-Methoxy-2-(2-morpholin-4-yl-ethoxy)-5-thiophen-2-yl-phenyl]-acryloyl}-benzenesulfonamide (Ex-81, 0.065 g, 0.12 mmol) was dissolved in tetrahydrofuran (5 mL) and 3 N HCl (1 mL) was added drop wise to the solution. The resulting yellow slurry was stirred in the dark at room temperature for 30 min. The precipitate was collected and dried in vacuo to yield 0.054 g (78%) of the title compound as a yellow solid, mp 235° C. (dec). 1H-NMR (300 MHz, DMSO-d6): δ 8.31–8.34 (m, 3H), 8.13 (d, 1H, J=15.0 Hz), 7.92–8.01 (m, 3H), 7.70 (d, 1H, J=4.0 Hz), 7.54 (m, 3H), 7.15–7.17 (m, 1H), 6.92 (s, 1H), 4.64 (brs, 2H), 4.03 (s, 5H), 3.72–3.79 (m, 4H), 3.56–3.60 (m, 4H). MS (ESI) m/z=529 ([M+H]+, 100%). Anal. Calcd. for C26H29ClN2O6S2: C, 55.26; H, 5.17; Cl, 6.27; N, 4.96; S, 11.35. Found: C, 55.31; H, 5.17; Cl, 6.32; N, 4.98; S, 11.20.

出典