HRID1395792

反应详情

EQUATION

反应方程式

HRID 1395792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 600 g 1-Cyanomethyl-4-phenylpiperazine in 1525 ml tetrahydrofuran was added dropwise to a suspension of 181 g LiAlH4 in 4.5 liters tetrahydrofuran. The mixture was refluxed 18 hours, cooled and added 181 ml water, 181 ml 15% NaOH, and 543 ml water. The mixture was filtered and concentrated to dryness on the rotovap and the residue distilled to give 470 g product, b0.1 117°-24°,m.50°-7°.

WORKUP

后处理

  1. temperatureThe mixture was refluxed 18 hours
  2. temperaturecooled
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated to dryness on the rotovap
  5. distillationthe residue distilled