반응 #1451478

반응 방정식

lithium hydroxide

lithium hydroxide

methanol

ethyl 4-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]-quinolin-2-carboxylate

HCl

→

4-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]quinolin-2-carboxylic acid hydrochloride

수율 98.0%

용매

water

반응 조건

후처리

1. 1
   workup.STIRRINGby stirring at 50° C. for 11 hours
2. 2
   온도The reaction mixture was cooled in an ice-bath
3. 3
   기타Then, crystals precipitated
4. 4
   여과were filtered out
5. 5
   세척washed with water
6. 6
   기타dried

실험 절차

An aqueous solution of 4N lithium hydroxide (3 ml) was added to a methanol solution (7 ml) of ethyl 4-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]-quinolin-2-carboxylate (1.5 g), followed by stirring at room temperature overnight. Then, water (10 ml) and aqueous solution (3 ml) of 4N lithium hydroxide were further added, followed by stirring at 50° C. for 11 hours. The reaction mixture was cooled in an ice-bath, and an aqueous solution (4 ml) of 6N—HCl was added thereto. Then, crystals precipitated were filtered out, washed with water and dried to obtain 4-[3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propoxy]quinolin-2-carboxylic acid hydrochloride (1.43 g, yield: 98%) as white powder.

출처