反应详情

温度

60 °C

To a suspension of 75 g (323 mmol) of 4-hydroxybenzenesulfonic acid sodium salt in 1350 ml of DMF, 20.67 g (517 mmol) of 60% oil suspended NaH are carefully added portionwise at r.t. To the mixture, 11.93 g (32.3 mmol) of tetrabutylammonium iodide and 50.13 ml (517 mmol) of (bromomethyl)-cyclopropane are added successively. After stirring for 25 h at 60° C., the reaction mixture is cooled to r.t. Precipitates are collected and washed with CH2Cl2 several times, and then recrystalized with mixed solvent (EtOH-H2O=2:1) to give the title compound as a colorless solid.

1. additionare carefully added portionwise at r.t
2. temperaturethe reaction mixture is cooled to r.t
3. customPrecipitates
4. customare collected
5. washwashed with CH2Cl2 several times
6. customrecrystalized with mixed solvent (EtOH-H2O=2:1)