反応 #2859

反応方程式

EtOAc

methyl iodide

sodium hydride

5-Chlorothieno[3,2-b]pyridine-2-sulfonic acid [1-(3-cyanobenzyl)-2-oxo-pyrrolidin-3-(S)-yl]-amide

→

title compound

5-Chlorothieno[3,2-b]pyridine-2-sulfonic acid [1-(3-cyanobenzyl)-2-oxo-pyrrolidin-3-(S)-yl]-methylamide

溶媒

DMF

反応条件

後処理

1. 1
   温度to warm to room temperature
2. 2
   その他the layers are separated
3. 3
   洗浄The organic layer is washed with 1N HCl, H2O, saturated NaHCO3 solution and saturated NaCl
4. 4
   乾燥The organic phase is then dried over MgSO4
5. 5
   ろ過filtered
6. 6
   濃縮concentrated

実験手順

5-Chlorothieno[3,2-b]pyridine-2-sulfonic acid [1-(3-cyanobenzyl)-2-oxo-pyrrolidin-3-(S)-yl]-amide (0.25 g, 0.56 mmol) is dissolved in 6 mL of DMF and cooled to 0° C. To the solution is added methyl iodide (0.40 g, 2.82 mmol) and sodium hydride (25 mg of a 60% dispersion in mineral oil, 0.62 mmol). The reaction mixture is allowed to warm to room temperature and is stirred for 2 h. At this time, the solution is diluted with and EtOAc and the layers are separated. The organic layer is washed with 1N HCl, H2O, saturated NaHCO3 solution and saturated NaCl. The organic phase is then dried over MgSO4, filtered and concentrated to give the title compound (0.25 g, 0.54 mmol) as a solid.

出典