反応 #60570

反応方程式

4-acetylamino-N-(2-diethylamino-ethyl)-2-methoxy-benzamide

cesium carbonate

iodomethane

→

[2-(4-Acetylamino-2-methoxy-benzoylamino)-ethyl]-diethyl-methyl-ammonium iodide

溶媒

dimethylformamide

反応条件

後処理

1. 1
   濃縮After concentration
2. 2
   その他by evaporation under vacuum, it
3. 3
   抽出extracted three times with 25 ml each of methylene chloride
4. 4
   その他The collected organic phase is dried
5. 5
   ろ過filtered
6. 6
   濃縮concentrated by evaporation, and 145 mg (32% of theory) of [2-(4-acetylamino-2-methoxy-benzoylamino)-ethyl]-diethyl-methyl-ammonium iodide with a melting point >300° C.
7. 7
   その他is obtained

実験手順

307 mg (1, mmol) of 4-acetylamino-N-(2-diethylamino-ethyl)-2-methoxy-benzamide is mixed in 8 ml of dimethylformamide with 358 mg (1.1 mmol) of cesium carbonate and 312 mg (2.2 mmol) of iodomethane, and it is heated under argon in a pressure vessel for 2.5 hours to a bath temperature of 80° C. After concentration by evaporation under vacuum, it is taken up in 25 ml of saturated sodium bicarbonate solution and extracted three times with 25 ml each of methylene chloride. The collected organic phase is dried, filtered and concentrated by evaporation, and 145 mg (32% of theory) of [2-(4-acetylamino-2-methoxy-benzoylamino)-ethyl]-diethyl-methyl-ammonium iodide with a melting point >300° C. is obtained.

出典