反应详情

温度

120 °C

A mixture of potassium acetate (16.9 g, 172 mmol) and cis-3-(toluene-4-sulfonyloxy)-cyclobutanecarboxylic acid methyl ester (9.8 g, 34 mmol; trans/cis=1:5) in dry DMF (50 mL) was heated to 120° C. for 21 h. DMF was partially distilled off (≈30 mL), water was added, and the mixture was extracted with EtOAc (6×50 mL). The combined organic layers were washed with water (2×), brine, dried over MgSO4, filtered and concentrated to give the title compound as brown oil, trans/cis=5:1 based on 1H NMR. The material thus obtained was used without further purification.

1. distillationDMF was partially distilled off (≈30 mL), water
2. additionwas added
3. extractionthe mixture was extracted with EtOAc (6×50 mL)
4. washThe combined organic layers were washed with water (2×), brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated