HRID549218

反应详情

EQUATION

反应方程式

HRID 549218 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound was prepared in a manner analogous to that of Step A of Example 1, using 4.9 grams (0.026 mole) of 2-{[(6-chloro-3-pyridyl)methyl]amino}ethan-1-ol, 3.6 grams (0.026 mole) of 4-methoxybenzaldehyde, 8.3 grams (0.039 mole) of sodium triacetoxyborohydride and 5.8 grams (0.052 mole) of magnesium sulfate in 200 mL of 1,2-dichloroethane. The crude product was purified with column chromatography on silica gel. Elution was accomplished using 100% methylene chloride and 100% diethyl ether as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 9.3 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 of Step A of Example 1
  2. customThe crude product was purified with column chromatography on silica gel
  3. washElution
  4. concentrationconcentrated under reduced pressure