반응 #735288

반응 방정식

lithium aluminum hydride

6-chloro-2'-propionylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline]

→

6-Chloro-2'-propylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] hydrochloride

용매

ether

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도The reaction mixture is heated
2. 2
   온도under reflux for four hours
3. 3
   온도cooled
4. 4
   기타quenched by the dropwise addition of saturated ammonium chloride solution (100 ml)
5. 5
   여과The mixture is filtered
6. 6
   workup.ADDITIONdiluted with ether
7. 7
   세척washed with water (2X), saturated sodium chloride solution
8. 8
   건조dried over anhydrous magnesium sulfate
9. 9
   여과After filtering
10. 10
    기타the solvent is removed
11. 11
    기타to yield an oil which
12. 12
    기타The salt is recrystallized from ethyl acetate/methanol
13. 13
    기타to yield the analytical sample as a white solid, mp 227°-228° (dec.)

실험 절차

To a refluxing suspension of lithium aluminum hydride (1.4 g) in tetrahydrofuran (100 ml) is slowly dropped 6-chloro-2'-propionylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (6.1 g) in tetrahydrofuran (50 ml). The reaction mixture is heated under reflux for four hours, cooled and quenched by the dropwise addition of saturated ammonium chloride solution (100 ml). The mixture is filtered, diluted with ether, washed with water (2X), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solvent is removed to yield an oil which is dissolved in ether and converted to the product hydrochloride salt (6.0 g, 90%). The salt is recrystallized from ethyl acetate/methanol to yield the analytical sample as a white solid, mp 227°-228° (dec.).

출처