HRID481420

反应详情

EQUATION

反应方程式

HRID 481420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium metal (0.754 mol) was dissolved in absolute ethanol (100 ml) and the resulting solution was added dropwise to a solution of methoxyacetamidine hydrochloride (0.703 mol) in ethanol (100 ml). After 15 minutes the reaction mixture was filtered and the filtrate was added to a solution of diethyl formylsuccinate (0.703 mol), which was prepared according to H. Nakao et al. Ann. Sankyo Res. Lab., 18, 33-37 (1966). The reaction was refluxed for 15 hours, cooled to room temperature and was then concentrated to obtain a crude solid. This solid was crystallized from isopropanol to obtain the title compound (43% yield), m.p. 142°-143° C.

WORKUP

后处理

  1. filtrationAfter 15 minutes the reaction mixture was filtered
  2. customwas prepared
  3. temperatureThe reaction was refluxed for 15 hours
  4. concentrationwas then concentrated
  5. customto obtain a crude solid
  6. customThis solid was crystallized from isopropanol