HRID522154

反应详情

EQUATION

反应方程式

HRID 522154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2,3-dicyanopropanoate (1.58 g, 10.38 mmol) in methanol (52 mL) and pyridine (2.52 mL, 31.14 mmol) was cooled to 10° C. in an ice bath. Benzenediazonium tetrafluoroborate was added portion-wise over 20 minutes at 10° C. and the reaction stirred at room temperature for 18 hours. The reaction was concentrated in vacuo and partitioned between DCM and water. The organic layer was dried over magnesium sulphate and concentrated in vacuo to afford the title compound (2.8 g, 28%). The crude product was taken on directly to the next step.

WORKUP

后处理

  1. concentrationThe reaction was concentrated in vacuo
  2. custompartitioned between DCM and water
  3. dry with materialThe organic layer was dried over magnesium sulphate
  4. concentrationconcentrated in vacuo