反応 #52982

反応方程式

1,4-Benzodioxan-6-carboxaldehyde

H2SO4

H2O2

→

6-hydroxy-1,4-benzodioxan

反応条件

後処理

1. 1
   その他evaporated
2. 2
   抽出extracted with CH2Cl2
3. 3
   乾燥The extract was dried (Na2SO4)
4. 4
   ろ過filtered
5. 5
   その他evaporated
6. 6
   その他The residue was purified by column chromatography (silica gel; eluent: hexane to hexane/EtOAc 3:1)

実験手順

1,4-Benzodioxan-6-carboxaldehyde (5.20 g) was dissolved in MeCH (60 mL) containing conc. H2SO4 (0.6 mL). At 0° C. an aqueous solution of 30% H2O2 (4.7 mL) was added to the mixture over 5 minutes. The mixture was warmed to room temperature, stirred an additional 18 h and evaporated. The residue was taken up with H2O and extracted with CH2Cl2. The extract was dried (Na2SO4), filtered and evaporated. The residue was purified by column chromatography (silica gel; eluent: hexane to hexane/EtOAc 3:1) to give 6-hydroxy-1,4-benzodioxan (3.85 g). ESMS: m/z 153 MH+.

出典