반응 #52982

반응 방정식

1,4-Benzodioxan-6-carboxaldehyde

H2SO4

H2O2

→

6-hydroxy-1,4-benzodioxan

반응 조건

후처리

1. 1
   기타evaporated
2. 2
   추출extracted with CH2Cl2
3. 3
   건조The extract was dried (Na2SO4)
4. 4
   여과filtered
5. 5
   기타evaporated
6. 6
   기타The residue was purified by column chromatography (silica gel; eluent: hexane to hexane/EtOAc 3:1)

실험 절차

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+.

출처