反应详情

温度

40 °C

5.61 g of 5-hydroxyhex-3-yn-2-one [prepared according to A. F. Thomas et al., Tet. Let. 27, 505, (1986)] in 50 ml of methylene chloride are added dropwise while stirring within 15 min. to a mixture of 11.42 g of thioacetic acid in 50 ml of methylene chloride and 100 ml of 2N sulphuric acid. After leaving to stand at room temperature for 2 hours the mixture is heated to 40° C. and stirred at 40° C. for a further 4 hrs. The reaction mixture is poured into 100 ml of H2O and extracted 2× with 100 ml of methylene chloride. The organic phases, dried over MgSO4, are concentrated and fractionally distilled in a high vacuum (65° C./0.2 mbar). There are obtained 5.7 g (67% of theory) of a yellow liquid.

1. customAfter leaving
2. extractionextracted 2× with 100 ml of methylene chloride
3. dry with materialThe organic phases, dried over MgSO4
4. concentrationare concentrated
5. distillationfractionally distilled in a high vacuum (65° C./0.2 mbar)
6. customThere are obtained 5.7 g (67% of theory) of a yellow liquid