HRID549227

反应详情

EQUATION

反应方程式

HRID 549227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

This compound was prepared in a manner analogous to that set forth in Step C of Example 1, using 6.0 grams (0.0193 mole) of 2-{[(6-chloro(3-pyridyl)methyl][(4-chlorophenyl)methyl]amino}ethan-1-ol, 2.4 grams (0.0203 mole) of thionyl chloride and four drops (catalyst) of pyridine in 75 mL of chloroform. The crude product was purified with column chromatography on silica gel. Elution was accomplished using 15% ethyl acetate in hexane then 30% ethyl acetate in hexane as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 5.7 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. customThis compound was prepared in a manner analogous to that set forth in Step C of Example 1
  2. customThe crude product was purified with column chromatography on silica gel
  3. washElution
  4. concentrationconcentrated under reduced pressure