反应 #1563873
ord-0fd8ff75caee430f8334662434a329f3
反应方程式
2-diazo-1-(thiophen-2-yl)ethanone
3,4,5,6-tetrachlorocyclohexa-3,5-diene-1,2-dione
→
(4,5,6,7-tetrachlorobenzo[d][1,3]dioxol-2-yl)(thiophen-2-yl)methanone
收率 43.7%
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度refluxed vigorously for 6 hours
- 2其他The solvent was then evaporated to dryness
- 3其他Evaporation of the solvent
实验过程
2-diazo-1-(thiophen-2-yl)ethanone (2.3 g, 0.0151 mol) and 3,4,5,6-tetrachlorocyclohexa-3,5-diene-1,2-dione (3.36 g, 0.0136 mol) were then combined in dry benzene (25 mL) and refluxed vigorously for 6 hours. The solvent was then evaporated to dryness, and the crude material was subjected to column chromatography using 100-200 mesh silica gel and 15% ethyl acetate-hexane solvent system. Evaporation of the solvent yielded (4,5,6,7-tetrachlorobenzo[d][1,3]dioxol-2-yl)(thiophen-2-yl)methanone as an orange solid (2.2 g, 43.4%).