反応 #46315

反応方程式

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

溶媒

Na2CO3

反応条件

後処理

1. 1
   温度The reaction mixture is refluxed for 4 days under argon
2. 2
   温度after cooling
3. 3
   抽出extracted with ethyl acetate
4. 4
   乾燥dried over anhydrous sodium sulphate
5. 5
   ろ過filtered
6. 6
   その他evaporated to dryness under reduced pressure
7. 7
   その他to be isolated

実験手順

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.

出典