تفاعل #365781

معادلة التفاعل

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

4-(4-pyridyl)benzoic acid

HOBt

WSC hydrochloride

→

title compound

المردود 95.7%

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

المردود 95.7%

المذيبات

DMF

triethylamine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling
2. 2
   تركيزconcentrated
3. 3
   workup.ADDITIONTo the residue was added ethyl acetate and sodium bicarbonate solution
4. 4
   أخرىThe organic layer was separated
5. 5
   غسيلwashed with water
6. 6
   استخلاصextracted with 1 N hydrochloric acid
7. 7
   استخلاصextracted with dichloromethane
8. 8
   أخرىThe extract was dried
9. 9
   تركيزconcentrated
10. 10
    أخرىthe residue was crystallized with ether

الإجراء التجريبي

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).

المصدر