HRID365566

反应详情

EQUATION

反应方程式

HRID 365566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8-[2,6-dichloro-3-[N-methyl-N-(phthalimidoacetyl)amino]benzyloxy]-2-methyl-4-(2-pyridylmethoxy)quinoline (750 mg), hydrazine monohydrate (117 mg) and ethanol was heated under reflex for 4 hours. The precipitate was removed by filtration and filtrate was evaporated in vacuo. The residue was dissolved with a mixture of chloroform and methanol (10:1, V/V), precipitate was removed by filtration and filtrate was evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with chloroform - methanol to afford 8-[3-(N-glycyl-N-methylamino)-2,6-dichlorobenzyloxy]-2-methyl-4-(2-pyridylmethoxy)quinoline (390 mg) as an amorphous powder.

WORKUP

后处理

  1. temperaturewas heated under reflex for 4 hours
  2. customThe precipitate was removed by filtration and filtrate
  3. customwas evaporated in vacuo
  4. dissolutionThe residue was dissolved with a mixture of chloroform and methanol (10:1, V/V), precipitate
  5. customwas removed by filtration and filtrate
  6. customwas evaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel eluting with chloroform - methanol