反応 #11762

反応方程式

5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzenesulfonamide

triethylamine

acetic acid 1-chlorocarbonyl-1-methyl-ethyl ester

hydrochloric acid

→

crude title compound

収率 111.5%

Acetic acid 2-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzenesulfonylamino)-1,1-dimethyl-2-oxo-ethyl ester

収率 111.5%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   抽出extracted with dichloromethane
3. 3
   乾燥dried over magnesium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo

実験手順

To a solution of 5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzenesulfonamide (0.10 g, 0.21 mmol) in dichloromethane (2 mL) was added triethylamine (0.033 mL, 0.23 mmol), 4-dimethylaminopyridine (5 mg, 0.04 mmol) and acetic acid 1-chlorocarbonyl-1-methyl-ethyl ester (0.037 mL, 0.25 mmol). The resulting reaction mixture was stirred at ambient temperature overnight, treated with 0.2 N hydrochloric acid extracted with dichloromethane dried over magnesium sulfate, filtered and concentrated in vacuo to give the crude title compound (0.140 g).

出典