HRID2107622

反应详情

EQUATION

反应方程式

HRID 2107622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a refluxing solution of diphenyl ether (250 ml) was added ethyl 2-ethoxycarbonyl-3-(4-methoxy-3-thienylamino)prop-2-enoate (25 g, 0.0836 mol) portionwise. On completion of the addition, refluxing was continued for a further 20 minutes. The reaction mixture was allowed to cool and then diluted with petroleum ether (b.p. 40°-60°) (400 ml) to give a dark brown solid. This was collected by filtration, washed with petroleum-ether (b.p. 40°-60°) (100 ml) and dried. The solid was recrystallized from DMF (30 ml) to give the title compound as a pale purple solid, 12.7 g, m.p. 244°-247°.

WORKUP

后处理

  1. additionOn completion of the addition
  2. temperaturerefluxing
  3. temperatureto cool
  4. customto give a dark brown solid
  5. filtrationThis was collected by filtration
  6. washwashed with petroleum-ether (b.p. 40°-60°) (100 ml)
  7. customdried
  8. customThe solid was recrystallized from DMF (30 ml)