HRID1702622

反应详情

EQUATION

反应方程式

HRID 1702622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 0.2 mole (34.8 g) of 1,3-dimethyl-2-oxoquinoxaline in 300 ml of dry tetrahydrofuran was added dropwise 0.24 mole (240 ml of 1 M) diborane in tetrahydrofuran. The solution was stirred one additional hour, then heated at its reflux temperature for one day. After cooling, about 40 ml of water was added, followed by 2 equivalents of 4 N hydrochloric acid. The solution was heated at reflux for one hour, then evaporated to provide a solid residue. The residue was dissolved in water. The solution was basified and then extracted with diethyl ether. The ether was dried, then evaporated to provide an oil. Distillation provides 1,3-dimethyl-1,2,3,4-tetrahydroquinoxaline, b.p. 85° C./0.1 mm of Hg. Analysis: Calculated for C10H14N2 :%C, 74.0; %H, 8.7; %N, 17.4; Found : %C, 74.2; %H, 8.9; %N, 17.3.

WORKUP

后处理

  1. temperatureheated at its
  2. temperaturereflux temperature for one day
  3. temperatureAfter cooling
  4. temperatureThe solution was heated
  5. temperatureat reflux for one hour
  6. customevaporated
  7. customto provide a solid residue
  8. extractionextracted with diethyl ether
  9. dry with materialThe ether was dried
  10. customevaporated
  11. customto provide an oil
  12. distillationDistillation