반응 #46315

반응 방정식

compound

(±)-cis-1,2-Dihydroxy-6-methoxy-3,3,14-trimethyl-1,2,3,14-tetrahydro-7H-benzo[b]chromeno[6,5-g][1,8]naphthyridin-7-one

2-butanone

→

(±)-cis-7-Methoxy-4,4,15-trimethyl-15,15c-dihydro-4H-benzo[b][1,3]-dioxolo[4′,5′:3,4]chromeno[6,5-g][1,8]naphthyridin-2,8[3aH]-dione

용매

Na2CO3

반응 조건

후처리

1. 1
   온도The reaction mixture is refluxed for 4 days under argon
2. 2
   온도after cooling
3. 3
   추출extracted with ethyl acetate
4. 4
   건조dried over anhydrous sodium sulphate
5. 5
   여과filtered
6. 6
   기타evaporated to dryness under reduced pressure
7. 7
   기타to be isolated

실험 절차

635.62 mg of N,N′-carbonyldiimidazole are added to a solution of 200 mg of the compound of Example 3 in 90 ml of 2-butanone. The reaction mixture is refluxed for 4 days under argon and then, after cooling, diluted with an aqueous 5% Na2CO3 solution (15 ml) and extracted with ethyl acetate. The organic solutions are combined, dried over anhydrous sodium sulphate, filtered and then evaporated to dryness under reduced pressure. Chromatography on silica gel (dichloromethane and then a gradient of methanol in dichloromethane of from 0.1 to 1.5%) allow 78 mg of the expected product to be isolated.

출처