HRID1583623

反应详情

EQUATION

反应方程式

HRID 1583623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An autoclave containing a mixture of 3 g of 9-fluoro-8-chloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid, 8 g of morpholine and 30 ml of hexamethylphosphoric triamide was immersed in an oil bath at 190° C. and reaction was continued for 5 hours. After completion of reaction, the reaction mixture was cooled to precipitate crystals which then were collected by filtration. The crystals thus obtained were recrystallized from dimethylformamide to give 0.77 g of 9-morpholino-8-chloro-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid. m.p. 271° to 274° C., white rhombic crystals.

WORKUP

后处理

  1. additionAn autoclave containing
  2. customwas immersed in an oil bath at 190° C.
  3. customreaction
  4. customAfter completion of reaction
  5. temperaturethe reaction mixture was cooled
  6. customto precipitate crystals which
  7. filtrationthen were collected by filtration
  8. customThe crystals thus obtained
  9. customwere recrystallized from dimethylformamide