HRID1033018

反应详情

EQUATION

反应方程式

HRID 1033018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2-methoxy-3-(2-amino-1-(R/S)hydroxyethyl)-5-ethyl-6-methylpyridine (345 mg, 1.64 mmol) in ethanol (5 mL) was added N-(carbethoxy)-phthalimide (373 mg, 1.70 mmol). The reaction was stirred for six hours as suspension dissolved. The solvent was evaporated and the viscous residue triturated with ethyl acetate/diethyl ether as product crystallized. By filtration 273 mg (49%) of pure product was collected, m.p. 134°-135° C. These mother liquors were flash chromatographed on silica gel and eluted with 20% ethyl acetate/80% hexane to give an additional 83 mg (15%) of product.

WORKUP

后处理

  1. dissolutiondissolved
  2. customThe solvent was evaporated
  3. customthe viscous residue triturated with ethyl acetate/diethyl ether as product
  4. customcrystallized
  5. filtrationBy filtration 273 mg (49%) of pure product
  6. customwas collected
  7. customchromatographed on silica gel
  8. washeluted with 20% ethyl acetate/80% hexane