반응 #2667

반응 방정식

5-iodo vanillin

boron tribromide

→

expected product

수율 66.2%

3-iodo-4,5-dihydroxy benzaldehyde

수율 66.2%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   농축was then concentrated
2. 2
   온도cooled to 0° C.
3. 3
   기타The crystallized product was separated out
4. 4
   세척washed with water
5. 5
   기타dried
6. 6
   기타crystallized from an isopropanol

실험 절차

37.2 g of 5-iodo vanillin (commercial) and 360 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 135 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for 16 hours at ambient temperature and was then concentrated, cooled to 0° C. and acidified. The crystallized product was separated out, washed with water, dried and crystallized from an isopropanol--water mixture (1-2 by volume) to obtain 23.4 g of the expected product.

출처