反应详情

To a flamed dried flask is added dry toluene (80 mL) and sodium hydride (60%, 33.5 mmol, 1.34 g). The reaction is cooled in a ice bath and a solution of ethyl 1,3 dithiane carboxylate (52 mmol, 10 g) and bromomethyl cyclopropane (62.4 mmol, 8.42 g) in DMF (24 mL) are added dropwise over 10 minutes. The ice bath is removed and the reaction is stirred for 18 h. Water is added (50 mL) and the organic layer is separated. The organic layer is washed with brine, dried (Na2SO4), and concentrated to a yellow oil (12 g, 92%). LC-ES/MS: 247.0 (M+1).

1. customTo a flamed dried flask
2. temperatureThe reaction is cooled in a ice bath
3. customThe ice bath is removed
4. additionWater is added (50 mL)
5. customthe organic layer is separated
6. washThe organic layer is washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated to a yellow oil (12 g, 92%)