HRID1415925

反应详情

EQUATION

反应方程式

HRID 1415925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 7-chloro-6-fluoro-1-(2,4-difluoro-5-nitrophenyl)-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate (3.0 g) was added to a mixture of 50 ml of dichloromethane, 30 ml of ethanol, and 2 ml of conc. hydrochloric acid together with 280 mg of 10% palladium on carbon whereupon hydrogenation was carried out overnight at room temperature. Pyridine (2 ml) was added to the reaction solution, which was concentrated in vacua. To the residue were added 80 ml of chloroform and 10 ml of distilled water. The chloroform layer was separated, dried over anhydrous magnesium sulfate and then concentrated in vacua. Ethanol (8 ml) was added to the residue whereupon the solution was allowed to stand at room temperature. The precipitate was collected by filtration and washed with ethanol and then with diisopropyl ether to give 1.95 grams of the title compound.

WORKUP

后处理

  1. concentrationwas concentrated in vacua
  2. additionTo the residue were added 80 ml of chloroform and 10 ml of distilled water
  3. customThe chloroform layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacua
  6. additionEthanol (8 ml) was added to the residue whereupon the solution
  7. customto stand at room temperature
  8. filtrationThe precipitate was collected by filtration
  9. washwashed with ethanol