반응 #1837268

반응 방정식

intermediate 19

7-hydroxy-3,4-dihydroisoquinolin-1(2H)-one

1,3-dibromopropane

K2CO3

→

7-(3-bromopropoxy)-3,4-dihydroisoquinolin-1(2H)-one

수율 63.3%

용매

EtOH

water

반응 조건

후처리

1. 1
   온도the solution was heated
2. 2
   온도to reflux
3. 3
   추출extracted with EtOAc
4. 4
   세척The combined EtOAc layers were washed with water, brine
5. 5
   건조dried over anhydrous Na2SO4
6. 6
   농축concentrated in vacuo
7. 7
   기타purified by flash chromatography on silica gel column (elution with PE/EtOAc=5:1)

실험 절차

A mixture of intermediate 19 (326 mg, 2 mmol), 1,3-dibromopropane (0.62 mL, 6 mmol) and anhydrous K2CO3 (276 mg, 2 mmol) was dissolved in 4 mL of EtOH and the solution was heated to reflux and stirred overnight. The mixture was diluted with water and extracted with EtOAc. The combined EtOAc layers were washed with water, brine, dried over anhydrous Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc=5:1) to give 7-(3-bromopropoxy)-3,4-dihydroisoquinolin-1(2H)-one (intermediate 20) (360 mg, 63%) as a white solid.

출처