HRID1649418

反应详情

EQUATION

反应方程式

HRID 1649418 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

42.5 g of 5-chloro-3,4-dihydrocarbostyril was suspended in 250 ml of dioxane and 44.3 g of NaBH4 was added to the suspension. Then 67 ml of acetic acid (d=1.05) was added dropwise to the mixture at room temperature. After heat-refluxing the resulting mixture for 2 hours the solvent was removed under reduced pressure. Water was added to the residue and insoluble materials were removed by filtration followed by washing with diethyl ether. The residue was extracted with diethyl ether, dried over anhydrous sodium sulfate and distilled under reduced pressure to obtain 36.0 g of 5-chloro-1,2,3,4-tetrahydroquinoline having a boiling point of 116° to 120° C./0.2 mmHg.

WORKUP

后处理

  1. temperatureAfter heat-refluxing the resulting mixture for 2 hours the solvent
  2. customwas removed under reduced pressure
  3. additionWater was added to the residue and insoluble materials
  4. customwere removed by filtration
  5. washby washing with diethyl ether
  6. extractionThe residue was extracted with diethyl ether
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationdistilled under reduced pressure