반응 #60570

반응 방정식

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

cesium carbonate

iodomethane

→

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

용매

dimethylformamide

반응 조건

후처리

1. 1
   농축After concentration
2. 2
   기타by evaporation under vacuum, it
3. 3
   추출extracted three times with 25 ml each of methylene chloride
4. 4
   기타The collected organic phase is dried
5. 5
   여과filtered
6. 6
   농축concentrated 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
   기타is obtained

실험 절차

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.

출처