反応 #43415

反応方程式

3,8-difluoro-4-methylidene-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one

tert-butanol water

sodium sulphite

→

solid

収率 97.0%

3,8-Difluoro-4-hydroxy-4-(hydroxymethyl)-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one

収率 97.0%

反応条件

後処理

1. 1
   workup.ADDITIONmix alpha (4.3 g) under argon
2. 2
   workup.STIRRINGAfter 10 minutes stirring the mixture
3. 3
   抽出was extracted with 20% methanol in dichloromethane (3×300 ml)
4. 4
   乾燥The organic extracts were dried over magnesium sulphate
5. 5
   その他evaporated

実験手順

A solution of 3,8-difluoro-4-methylidene-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one (631 mg, 2.9 mmol) in tert-butanol/water (30 ml/30 ml) was treated with AD mix alpha (4.3 g) under argon. After 18 hours stirring the reaction mixture was treated with saturated sodium sulphite solution (30 ml). After 10 minutes stirring the mixture was extracted with 20% methanol in dichloromethane (3×300 ml). The organic extracts were dried over magnesium sulphate and evaporated affording a white solid (710 mg, 97%).

出典