反応 #77811

反応方程式

5-(2-bromo-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

potassium thioacetate

→

5-(2-acetylthio-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

収率 91.4%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   workup.DISTILLATIONSolvent was distilled off under reduced pressure, and ethyl acetate
2. 2
   workup.ADDITIONwas added to the residue, which
3. 3
   洗浄was washed with water and saturated brine in sequence
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONSolvent was distilled off under reduced pressure
6. 6
   その他the residue obtained
7. 7
   その他was crystallized from hexane-ethyl acetate
8. 8
   ろ過the crystals were collected by filtration

実験手順

To 1.00 g of 5-(2-bromo-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 80 ml of tetrahydrofuran and 368 mg of potassium thioacetate under an atmosphere of argon, and the mixture was stirred for 6 hours at room temperature. Solvent was distilled off under reduced pressure, and ethyl acetate was added to the residue, which was washed with water and saturated brine in sequence and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was crystallized from hexane-ethyl acetate, then the crystals were collected by filtration to obtain 904 mg of 5-(2-acetylthio-2-carbamoylethyl)-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as light brown crystals.

出典