HRID847778

反应详情

EQUATION

反应方程式

HRID 847778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 9.5 g of 5,8-dihydro-5-ethyl-8-oxofuro-[3,2-b]-1,8-naphthyridine-2,7-dicarboxylic acid (Compound X where R1 =C2H5), 0.8 g of copper powder and 250 ml of diethyl phthalate was heated at 250° to 260° C. for 25 minutes. After cooling, the reaction mixture was separated by partitioning between chloroform and aqueous potassium carbonate solution. The aqueous layer which separated out was acidified with hydrochloric acid and extracted with chloroform. The extract was treated with charcoal, and washed with water, dried and concentrated. The crystals precipitated by adding ethanol were collected by filtration to obtain 4.2 g of 5,8-dihydro-5-ethyl-8-oxofuro[3,2-b]-1,8-naphthyridine-7-carboxylic acid (Compound Ia where R1 =C2H5).

WORKUP

后处理

  1. temperaturewas heated at 250° to 260° C. for 25 minutes
  2. temperatureAfter cooling
  3. customthe reaction mixture was separated
  4. customby partitioning between chloroform and aqueous potassium carbonate solution
  5. customThe aqueous layer which separated out
  6. extractionextracted with chloroform
  7. additionThe extract was treated with charcoal
  8. washwashed with water
  9. customdried
  10. concentrationconcentrated
  11. customThe crystals precipitated
  12. additionby adding ethanol
  13. filtrationwere collected by filtration