反应详情

To 1,2-dimethoxyethane (25 mL) suspension of 0.16 g of dichlorobis(triphenylphosphine)palladium(II) were added 0.12 g of triphenylphosphine, 0.01 g of sodium borohydride, 5.53 g of potassium tert-butoxide and 3.48 g of tert-butyl cyanoacetate, which was then stirred at room temperature for 10 minutes. Thereto was added 5.00 g of 5-bromobenzothiophene, which was then refluxed for 2 hours. After to the reaction mixture was added 15 mL of water, the pH was adjusted to 1 with 2 mL of hydrochloric acid. The precipitate was collected by filtration to provide 5.69 g of tert-butyl 2-(1-benzothiophen-5-yl)-2-cyanoacetate as pale yellow solid form.

1. temperaturewas then refluxed for 2 hours
2. filtrationThe precipitate was collected by filtration