반응 #735275

반응 방정식

6',7'-dimethoxy-2'-ethoxycarbonylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline]

potassium hydroxide

n-propanol

→

product

수율 81.0%

6',7'-Dimethoxyspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] maleate

수율 81.0%

용매

water

water

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도under reflux for four hours
3. 3
   기타Removal of the solvent under reduced pressure
4. 4
   기타yields an oil which
5. 5
   추출extracted with chloroform
6. 6
   세척The combined organic phases are washed with water, saturated sodium chloride solution
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   여과After filtering
9. 9
   기타the solvent is removed

실험 절차

A mixture of 6',7'-dimethoxy-2'-ethoxycarbonylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (4.2 g), potassium hydroxide (7.0 g) and water (7.0 ml) in n-propanol (150 ml) is heated under reflux for four hours. Removal of the solvent under reduced pressure yields an oil which is stirred in water (300 ml) and then extracted with chloroform. The combined organic phases are washed with water, saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solvent is removed to yield 3.1 g (81%) of product as an oil which is dissolved in ether and converted to the maleate salt (1.9 g), mp 165°-167°. The material is twice recrystallized from ethyl acetate/methanol to yield a white solid (1.4 g), mp 180°-181° (dec.)

출처