반응 #62747

반응 방정식

water

ethylcyanoacetate

7,8-dimethoxy-5-formyl-2H-1-benzopyran

piperidine

→

orange solid

수율 66.9%

Ethyl 2-cyano-3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)propenoate

수율 66.9%

용매

benzene

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to cool
3. 3
   추출The solution was extracted successively with water (200 mL), 0.5N hydrochloric acid (200 mL), saturated sodium bicarbonate solution (200 mL), H2O (200 mL)
4. 4
   건조dried over magnesium sulfate
5. 5
   기타The volatiles were removed under reduced pressure

실험 절차

A mixture of ethylcyanoacetate (11.3 g, 0.1 mole), 7,8-dimethoxy-5-formyl-2H-1-benzopyran (22.0 g, 0.1 mole), piperidine (1.02 g, 0.01 mole) and acetic acid (0.36 g, 0.006 mole) in benzene (100 mL) was heated at reflux for 5 hr with azeotropic removal of water and allowed to cool. The solution was extracted successively with water (200 mL), 0.5N hydrochloric acid (200 mL), saturated sodium bicarbonate solution (200 mL), H2O (200 mL) and dried over magnesium sulfate. The volatiles were removed under reduced pressure to give 21.1 g (66.9%) of an orange solid, mp 104.5°-107.5° C.

출처