تفاعل #77811

معادلة التفاعل

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

potassium thioacetate

→

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

المردود 91.4%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر