반응 #40717
ord-7a8b9422f4634db6947a7b29d86ba228
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타During the reaction
- 2기타After that, EtOH was evaporated off
- 3기타the resulting oil was dried in vacuum
- 4기타Trituration with ether (15 mL) gave light brown solids, which
- 5기타were removed by filtration
- 6세척washed with ether
- 7workup.DISSOLUTIONThe solids then re-dissolved in CHCl3
- 8여과filtered
- 9기타After evaporation of the solvent
- 10기타light brown solids were obtained (0.35 g, 50%)
실험 절차
1-Azido-5-chloro-2,4-dimethoxy-benzene (0.4 g, 1.9 mmol), 3-(4-Fluoro-phenyl)-3-oxo-propionic acid methyl ester (0.42 g, 2.2 mmol) and sodium ethoxide in EtOH (70 mg of sodium in 15 mL EtOH) were refluxed for 3 hours. During the reaction, the solution turned brown from dark green. After that, EtOH was evaporated off and the resulting oil was dried in vacuum. Trituration with ether (15 mL) gave light brown solids, which were removed by filtration and washed with ether. The solids then re-dissolved in CHCl3 and filtered. After evaporation of the solvent, light brown solids were obtained (0.35 g, 50%).