반응 #735279

반응 방정식

water

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

potassium hydroxide

water

→

product

수율 137.3%

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

수율 137.3%

용매

n-propanol

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 a solid which
5. 5
   추출extracted with ether
6. 6
   추출The combined ether extract
7. 7
   세척is washed with 3 N hydrochloric acid and basified with saturated sodium carbonate solution
8. 8
   추출The material which separates is extracted with ether
9. 9
   세척washed with saturated sodium chloride solution
10. 10
    건조dried over anhydrous magnesium sulfate
11. 11
    여과After filtering
12. 12
    기타the solvent is removed

실험 절차

A mixture of 6-chloro-2'-phenoxycarbonylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (25.0 g), potassium hydroxide (25 g) and water (25 ml) in n-propanol (250 ml) is heated under reflux for four hours. Removal of the solvent under reduced pressure yields a solid which is stirred with water (500 ml) and extracted with ether. The combined ether extract is washed with 3 N hydrochloric acid and basified with saturated sodium carbonate solution. The material which separates is extracted with ether, washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solvent is removed to yield product as a solid (13.5 g, 78%). A 4.0 g portion of the solid is dissolved in ether and converted to the product hydrochloride salt (4.3 g). An analytical sample is twice recrystallized from ethyl acetate/methanol, mp 238°-239° (dec).

출처