HRID64905

反应详情

EQUATION

反应方程式

HRID 64905 的结构方程式

PROCEDURE

实验过程

7-Bromo-9-(1,1-ethylenedioxy)ethyl-6,9-dihydroxy-5,7,8,9,10,12-hexahydronaphthacene-5,12-dione (571 mg) prepared in the foregoing step and N,N-dimethylethylenediamine (10 ml) were subjected to reaction in a nitrogen stream while cooling with ice for 1 hour. Excess of the N,N-dimethylethylenediamine was eliminated by distillation under reduced pressure. The residue was dissolved in dichloromethane (2 ml) and ether (4 ml) was added thereto, whereby 7-(2-dimethylaminoethyl)amino-9-(1,1-ethylenedioxy)ethyl-6,9-dihydroxy-5,7,8,9,10,12-hexahydronaphthacene-5,12-dione was obtained as yellow crystals (124 mg). M.P., 192°-196° C.

WORKUP

后处理

  1. customwere subjected to reaction in a nitrogen stream
  2. temperaturewhile cooling with ice for 1 hour
  3. distillationExcess of the N,N-dimethylethylenediamine was eliminated by distillation under reduced pressure
  4. dissolutionThe residue was dissolved in dichloromethane (2 ml)
  5. additionether (4 ml) was added