HRID259805

反应详情

EQUATION

反应方程式

HRID 259805 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Two dropping funnels are used for simultaneous dropwise addition of a solution of 35.5 g (0.2 mol) of methyl 3-amino-2-chloro-2-pentenoate and 31.5 g (0.7 mol) of formamide in 150 ml of methanol with stirring to 90.3 ml of a 30% strength sodium methylate solution in methanol at room temperature. The mixture is heated slowly to the reflux temperature and left at this for 10 h. After the mixture has cooled, dry HCl gas is passed through the solution until the pH is 3. Evaporation of the solvent is followed by extraction with butanone, drying and evaporation in a rotary evaporator. Yield: 87% [HPLC]

WORKUP

后处理

  1. temperatureThe mixture is heated slowly to the reflux temperature
  2. temperatureAfter the mixture has cooled
  3. customEvaporation of the solvent
  4. extractionis followed by extraction with butanone
  5. customdrying
  6. customevaporation
  7. customin a rotary evaporator