반응 #429633

반응 방정식

sodium bicarbonate

6-amino-1,2,3,4-tetrahydrodibenzofuran

2,5-hexanedione

water

→

6-(2,5-dimethylpyrol-1-yl)-1,2,3,4-tetrahydrodibenzofuran

수율 72.1%

용매

ethanol

반응 조건

후처리

1. 1
   온도was refluxed for 1 hour
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The extract was washed with brine
4. 4
   건조dried over sodium sulfate
5. 5
   기타evaporated in vacuo
6. 6
   기타The residue was purified by column chromatography on silica gel
7. 7
   기타the obtained oil was crystallized from a mixture of ethanol and water

실험 절차

A mixture of 6-amino-1,2,3,4-tetrahydrodibenzofuran (230 mg), 2,5-hexanedione (145 mg) and conc. hydrochloric acid (1 drop) in ethanol (3 ml) was refluxed for 1 hour and poured into water. The mixture was neutralized with aqueous saturated sodium bicarbonate and extracted with ethyl acetate. The extract was washed with brine, dried over sodium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel and the obtained oil was crystallized from a mixture of ethanol and water to give 6-(2,5-dimethylpyrol-1-yl)-1,2,3,4-tetrahydrodibenzofuran (235 mg).

출처