반응 #62746

반응 방정식

sodium methoxide

3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile

→

yellow oil

수율 62.2%

3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-dimethoxymethylpropanenitrile

수율 62.2%

용매

water

methanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 24 hr
3. 3
   온도to cool
4. 4
   추출The resultant mixture was extracted with toluene (1×200 mL and 2×100 mL)
5. 5
   추출The combined toluene portions were extracted with water (3×100 mL)
6. 6
   건조dried over magnesium sulfate
7. 7
   농축The toluene solution was concentrated
8. 8
   기타leaving a brown oil which
9. 9
   workup.DISTILLATIONwas distilled under reduced pressure

실험 절차

A mixture of sodium methoxide (8.86 g, 0.164 mole), and 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (Example 37A, 23.1 g, 0.080 mole) in methanol (60 mL) was heated at reflux for 24 hr, allowed to cool and diluted with water (200 mL). The resultant mixture was extracted with toluene (1×200 mL and 2×100 mL). The combined toluene portions were extracted with water (3×100 mL) and dried over magnesium sulfate. The toluene solution was concentrated leaving a brown oil which was distilled under reduced pressure to give 15.9 g (62%) of a yellow oil which was used without further purification.

출처