反応 #43434

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 82.0%

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

収率 82.0%

反応条件

後処理

1. 1
   workup.ADDITIONmix alpha/beta (0.75 g/0.75 g)
2. 2
   抽出After 10 minutes the mixture was extracted with 20% methanol in dichloromethane (3×200 ml)
3. 3
   濃縮The aqueous phase was concentrated (to ca 20 ml)
4. 4
   抽出further extracted with 20% methanol in dichloromethane (3×200 ml)
5. 5
   その他The organic extracts were dried
6. 6
   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 (219 mg, 1 mmol) in tert-butanol/water (10 ml/10 ml) was treated with AD mix alpha/beta (0.75 g/0.75 g). After 6 hours the reaction mixture was treated with saturated sodium sulphite solution (10 ml). After 10 minutes the mixture was extracted with 20% methanol in dichloromethane (3×200 ml). The aqueous phase was concentrated (to ca 20 ml) and further extracted with 20% methanol in dichloromethane (3×200 ml). The organic extracts were dried and evaporated affording a white solid (206 mg, 82%).

出典