反应详情

温度

60 °C

Under argon and with stirring, 1.5 g (9.02 mmol) of 8-thiochromanol are dissolved in 5 cm3 of dimethylformamide (DMF). 3.74 g (27.06 mmol) of K2CO3 are added and then 1.94 g (9.92 mmol) of ethyl 4-bromobutyrate dissolved in 6 cm3 of DMF are added dropwise. The mixture is heated at 60° C. for 5 hours. The DMF is evaporated off. The residue is taken up in H2O. The product is extracted with CH2Cl2 and then dried over MgSO4. Purification over a silica column (eluant: ether/petroleum ether 3: 7) yields 2.48 g of the title compound (white solid).

1. additionare added dropwise
2. customThe DMF is evaporated off
3. extractionThe product is extracted with CH2Cl2
4. dry with materialdried over MgSO4
5. customPurification over a silica column (eluant: ether/petroleum ether 3: 7)