HRID465111

反应详情

EQUATION

反应方程式

HRID 465111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A 0.2 g portion of α-ethylidene 3-pyridine acetonitrile and 0.315 ml of t-butoxy-bis-dimethylaminomethane were dissolved in tetrahydrofuran and stirred at 20° C. for 20 hours. The solvent was removed at reduced pressure and the orange oil was purified by chromatography, eluting with ethyl acetate:hexane (10:3). The eluate was concentrated to a solid which was recrystallized from methylene chloride-hexane, giving α-[3-(dimethylamino)-2-propenylidene]-3-pyridineacetonitrile as yellow crystals, mp 117°-120° C.

WORKUP

后处理

  1. customThe solvent was removed at reduced pressure
  2. customthe orange oil was purified by chromatography
  3. washeluting with ethyl acetate:hexane (10:3)
  4. concentrationThe eluate was concentrated to a solid which
  5. customwas recrystallized from methylene chloride-hexane