반응 #2495251

반응 방정식

4,4-dimethyl-2-[3-(4-methyl-piperazin-1-yl)-phenyl]-1,2,3,4-tetrahydro-quinoline-6-carboxylic acid methyl ester

sodium hydroxide

hydrochloric acid

→

4,4-dimethyl-2-[3-(4-methyl-piperazin-1-yl)-phenyl]-1,2,3,4-tetrahydro-quinoline-6-carboxylic acid

수율 99.7%

용매

methanol

tetrahydrofuran

water

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate (2×50 mL)
2. 2
   세척washed with water
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   농축concentrated in vacuo

실험 절차

To a stirred mixture solution of 4,4-dimethyl-2-[3-(4-methyl-piperazin-1-yl)-phenyl]-1,2,3,4-tetrahydro-quinoline-6-carboxylic acid methyl ester (610 mg, 1.49 mmol) in methanol (7.5 mL) and tetrahydrofuran (15 mL) was added 30% sodium hydroxide in water (7.5 mL). The reaction mixture was stirred at 60° C. for 16 h. The mixture was neutralized with a 3 N aqueous hydrochloric acid solution and extracted with ethyl acetate (2×50 mL), washed with water, dried over anhydrous sodium sulfate and then concentrated in vacuo to afford 4,4-dimethyl-2-[3-(4-methyl-piperazin-1-yl)-phenyl]-1,2,3,4-tetrahydro-quinoline-6-carboxylic acid (564 mg, 99%) as a light white solid which was used for next step without further purification: MS (ESI) M+1=380.2.

출처