HRID1597987

反应详情

EQUATION

反应方程式

HRID 1597987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(6-Chloro-2,3-dihydro-indol-1-yl)-7-nitro-quinazoline hydrochloride (2.16 g, 5.90 mmol) was slurried in 250 mL of ethanol containing 0.21 g of 10% paladium on carbon and treated with ammonium formate (1.68 g, 26.6 mmol). After 16 hours the mixture was filtered through celite and evaporated in vacuo to a residue. This was dissolved in chloroform, filtered and washed with sodium bicarbonate and brine then dried with magnesium sulfate, filtered and evaporated in vacuo to give crude product which was recrystallized from 50% aqueous ethanol. The solid was dissolved in methanol containing anhydrous hydrogen chloride and poured into ether to yield the title compound after filtration and drying in vacuo; 0.687 g (35%) M.P. 282°-283° C.

WORKUP

后处理

  1. filtrationAfter 16 hours the mixture was filtered through celite
  2. customevaporated in vacuo to a residue
  3. dissolutionThis was dissolved in chloroform
  4. filtrationfiltered
  5. washwashed with sodium bicarbonate and brine
  6. dry with materialthen dried with magnesium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customto give crude product which
  10. customwas recrystallized from 50% aqueous ethanol
  11. dissolutionThe solid was dissolved in methanol containing anhydrous hydrogen chloride
  12. additionpoured into ether