HRID543547

反应详情

EQUATION

反应方程式

HRID 543547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium aluminum hydride (1 g.) was dissolved in 100 ml. of anhydrous diethyl ether. To the stirred solution was added over a period of fifteen minutes a solution of 6a,7,8,9-tetrahydro-5-[(2,6-dimethoxyphenyl)methyl]pyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-one (1 g., 0.003 mole) in 50 ml. of dry tetrahydrofuran. The reaction mixture was refluxed for eighteen hours and was worked up by adding wet ether, filtering, drying and evaporating in vacuo. The residue (m.p. 110°-112° C.) was dissolved in ethanol and treated with diethyl ether saturated with hydrogen chloride. The separated solid was recrystallized from methanol to afford 0.7 g. (67% yield) of the title compound as the hydrochloride salt, m.p. 211°-213° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for eighteen hours
  2. filtrationfiltering
  3. customdrying
  4. customevaporating in vacuo
  5. dissolutionThe residue (m.p. 110°-112° C.) was dissolved in ethanol
  6. additiontreated with diethyl ether saturated with hydrogen chloride
  7. customThe separated solid was recrystallized from methanol
  8. customto afford 0.7 g