HRID1195708

反应详情

EQUATION

反应方程式

HRID 1195708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10 ml of chloroform were dissolved 1.2 g of 4-(3-chloro-2-hydroxypropy)-1-diphenylmethylpiperazine prepared in Example 23-(b) and 220 mg of 5-mercaptoquinoline, and 311 mg of DBU was further added thereto. Afterward, the liquid was allowed to stand at room temperature for 12 days. The reaction liquid was poured into 20 ml of water and was then extracted twice with methylene chloride. The resultant organic layer was separated, then dried with an anhydrous Glauber's salt, and was distilled off under reduced pressure. The resultant residue was purified through a silica gel chromatograph (an AcOEt effluent solvent was used) in order to obtain 130 mg of the desired compound.

WORKUP

后处理

  1. additionwas further added
  2. customThe reaction liquid
  3. extractionwas then extracted twice with methylene chloride
  4. customThe resultant organic layer was separated
  5. dry with materialdried with an anhydrous Glauber's salt
  6. distillationwas distilled off under reduced pressure
  7. customThe resultant residue was purified through a silica gel chromatograph (an AcOEt effluent solvent