反応 #1095065

反応方程式

hydrochloric acid

2-[2-(6-fluorobenzo[b]thiophen-5-yl)ethoxy]-acetic acid

methylene chloride

oxalyl chloride

N,N-dimethylformamide

→

N,N-diethyl-2-[2-(6-fluorobenzo[b]thiophen-5-yl)ethoxy]acetamide

溶媒

Water

反応条件

後処理

1. 1
   その他the organic layer is separated
2. 2
   洗浄The organic layer is washed with saturated aqueous solution of sodium chloride
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent is distilled off under reduced pressure

実験手順

In 10 mL of methylene chloride is dissolved 1.00 g of 2-[2-(6-fluorobenzo[b]thiophen-5-yl)ethoxy]-acetic acid. The solution is cooled to 5° C., 0.55 g of oxalyl chloride and 0.1 mL of N,N-dimethylformamide are added thereto, and the resulting mixture is stirred at ambient temperature for 2 hours. Water is added to the reaction mixture, pH is adjusted to 1.0 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. Thus, 1.24 g of N,N-diethyl-2-[2-(6-fluorobenzo[b]thiophen-5-yl)ethoxy]acetamide is obtained as an oily product.

出典