반응 #735285

반응 방정식

dimethylformamide

spiro[benzofuran-2(3H),4'(2'H)-isoquinoline]

sodium bicarbonate

chloroacetonitrile

→

2'-Cyanomethylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline]

용매

water

반응 조건

후처리

1. 1
   온도the mixture is heated to 70° for four hours
2. 2
   기타The dimethylformamide is evaporated
3. 3
   기타to give an oil, which
4. 4
   추출extracted with ether/dichloromethane
5. 5
   추출The organic extract
6. 6
   세척is washed with water (2X), saturated sodium chloride solution
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   여과After filtering
9. 9
   기타the solvents are evaporated to an oil which
10. 10
    기타For analysis, a sample is recrystallized twice from hexane/acetone
11. 11
    기타to yield platelets

실험 절차

To dry dimethylformamide is added spiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (11.0 g), sodium bicarbonate (8.4 g) and chloroacetonitrile (6.8 g) and the mixture is heated to 70° for four hours. The dimethylformamide is evaporated to give an oil, which is stirred with water (300 ml) for 15 minutes and then extracted with ether/dichloromethane. The organic extract is washed with water (2X), saturated sodium chloride solution and then dried over anhydrous magnesium sulfate. After filtering, the solvents are evaporated to an oil which solidifies to the product (10.6 g), 83%), as an off-white solid upon trituration with petroleum ether/ether. For analysis, a sample is recrystallized twice from hexane/acetone to yield platelets.

출처