HRID2301993

反应详情

EQUATION

反应方程式

HRID 2301993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of [1-ethyl-7-(3-guanidino-propoxy)-2-oxo-1,2-dihydro-quinolin-3-yl]-acetic acid trifluoroacetate (400 mg, 0.87 mmol) in 20 ml of methyl alcohol and 0.4 g of 10% Pd/C was hydrogenated under 50 psi of hydrogen for 3 days. The reaction mixture was filtered through diatomaceous earth and the filtrate concentrated in vacuo to a residue which was dissolved in 10 ml of hot acetic acid and hydrogenated over 0.4 g of 10% Pd/C for 3 days. The reaction mixture was filtered through diatomaceous earth and the filter cake washed with hot methyl alcohol. The combined filtrates were evaporated in vacuo to a residue of oil and solid. The residue was purified by chromatography on a reverse phase column to afford 57 mg of the title compound as a pale yellow solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through diatomaceous earth
  2. concentrationthe filtrate concentrated in vacuo to a residue which
  3. dissolutionwas dissolved in 10 ml of hot acetic acid
  4. filtrationThe reaction mixture was filtered through diatomaceous earth
  5. washthe filter cake washed with hot methyl alcohol
  6. customThe combined filtrates were evaporated in vacuo to a residue of oil and solid
  7. customThe residue was purified by chromatography on a reverse phase column