HRID417093

反应详情

EQUATION

反应方程式

HRID 417093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The suspension of 0.64 g (2.23 mmol) (6-benzyloxy-pyridin-3-yloxy)-acetic acid ethyl ester and 0.064 g 10% palladium on charcoal was hydrogenated for 1 h at 1.7 bar. The reaction mixture was filtered over Dicalite Speed Plus, washed with ethanol and the filtrate was treated with silica gel and evaporated. The residue was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) with a gradient from heptane:ethyl acetate (100:0 to 0:100) followed by ethyl acetate:methanol (100:0 to 50:50) to give the product as a colorless solid (91%). MS (Turbo Spray): m/z=198.0 [M+H].

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over Dicalite Speed Plus
  2. washwashed with ethanol
  3. additionthe filtrate was treated with silica gel
  4. customevaporated
  5. customThe residue was purified by silica gel chromatography