반응 #365781

반응 방정식

1-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride

4-(4-pyridyl)benzoic acid

HOBt

WSC hydrochloride

→

title compound

수율 95.7%

1-(6-Chloronaphthalene-2-sulfonyl)-4-[4-(4-pyridyl)benzoyl]piperazine

수율 95.7%

용매

DMF

triethylamine

반응 조건

후처리

1. 1
   온도cooling
2. 2
   농축concentrated
3. 3
   workup.ADDITIONTo the residue was added ethyl acetate and sodium bicarbonate solution
4. 4
   기타The organic layer was separated
5. 5
   세척washed with water
6. 6
   추출extracted with 1 N hydrochloric acid
7. 7
   추출extracted with dichloromethane
8. 8
   기타The extract was dried
9. 9
   농축concentrated
10. 10
    기타the residue was crystallized with ether

실험 절차

To a solution of 1-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (90 mg), 4-(4-pyridyl)benzoic acid (52 mg), triethylamine (35 mg) and HOBt (39 mg) in DMF (10 ml) was added WSC hydrochloride (55 mg) under ice-cooling and the solution was stirred at room temperature 4 hours and concentrated. To the residue was added ethyl acetate and sodium bicarbonate solution. The organic layer was separated, washed with water, and extracted with 1 N hydrochloric acid. The extract was made alkaline with sodium hydroxide solution and extracted with dichloromethane. The extract was dried and concentrated, and the residue was crystallized with ether to give colorless crystals of the title compound (122 mg).

출처