HRID1447399

反应详情

EQUATION

反应方程式

HRID 1447399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the suspension of 12.8 g of 2-methyl-3,4-dioxo-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine in 460 ml of tetrahydrofuran, 200 ml of 1-molar diborane in tetrahydrofuran are added while stirring and cooling with ice. The mixture is refluxed for one hour, again cooled and combined with 25 ml of acetic acid. It is evaporated, the residue taken up in 50 ml of 30% aqueous sodium hydroxide and the mixture extracted with methylene chloride. The extract is dried, evaporated, the residue dissolved in diethyl ether, the solution filtered and the filtrate evaporated, to yield the 2-methyl-1,3,4,14b-tetrahydro-10H--pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine.

WORKUP

后处理

  1. additionare added
  2. temperaturecooling with ice
  3. temperatureThe mixture is refluxed for one hour
  4. temperatureagain cooled
  5. customIt is evaporated
  6. extractionthe mixture extracted with methylene chloride
  7. customThe extract is dried
  8. customevaporated
  9. dissolutionthe residue dissolved in diethyl ether
  10. filtrationthe solution filtered
  11. customthe filtrate evaporated