反応 #49708

反応方程式

N-(4'-iodophenyl)-2-amino octane

acetic acid

acetic anhydride

→

N-acetyl-N-2-octyl-4-iodoaniline

収率 70.0%

溶媒

ether

反応条件

後処理

1. 1
   その他The reaction flask was immersed in an oil bath
2. 2
   温度to cool
3. 3
   洗浄washed with water (2×50 ml), saturated aqueous sodium bicarbonate (4×50 ml), water (2×50 ml) and brine (50 ml)
4. 4
   乾燥dried (Na2SO4)
5. 5
   ろ過filtered
6. 6
   その他evaporated in vacuo

実験手順

A flask containing N-(4'-iodophenyl)-2-amino octane (1.50 g, 4.5 mmol) was charged with acetic acid (15 ml) and acetic anhydride (15 ml). The reaction flask was immersed in an oil bath which was warmed to 70° C. over a period of 0.5 hr. After stirring for 19 hrs, the reaction was allowed to cool, diluted with ether (200 ml), washed with water (2×50 ml), saturated aqueous sodium bicarbonate (4×50 ml), water (2×50 ml) and brine (50 ml), dried (Na2SO4), filtered, and evaporated in vacuo. Flash column chromatography (silica, 1:4; EtOAc:hexanes) provided N-acetyl-N-2-octyl-4-iodoaniline (1.48 g, 70%) as a white solid. Mp 60°-62° C.

出典