HRID1927233

反应详情

EQUATION

反应方程式

HRID 1927233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of THF (7 mL) and NaH (210 mg/60% in oil) was added dropwise a solution of THF (7 mL) and 4-cyano-2-diaminomethylene-butyric acid ethyl ester (0.55 g) described in Manufacturing Example 10-2-1, which was refluxed for 19 hours and 20 minutes. The reaction solution was poured into ice water and then extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, after which the solvent was evaporated under a reduced pressure to obtain the crude titled compound (0.19 g).

WORKUP

后处理

  1. temperaturewas refluxed for 19 hours and 20 minutes
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. customafter which the solvent was evaporated under a reduced pressure