HRID1111390

反应详情

EQUATION

反应方程式

HRID 1111390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred mixture of 6-methoxy-4-methyl-8nitro-5-(4-phenylbutoxy) quinoline (3.7 g, 0.01 mol), degreased 40mesh Fe filings (10 g), H2O (40 ml), HOAc (8 ml) and Bu2O (8 ml) was heated at 80°-100° C. for 2.5 h, allowed to cool and filtered. The solid was thoroughly extracted with Et2O and the extract was dried (Na2SO4), treated with carbon and concentrated to an oil. Extraction of the latter with pet ether and cooling the extract gave 2.2 g (66%) of 8-amino-6methoxy-4-methyl-5-(4-phenylbutoxy)quinoline as yellow-green crystals, mp 59°-59.5° C. Recrystallization from pet ether afforded the analytical sample as yellow crystals, mp 60°-61° C.

WORKUP

后处理

  1. temperaturewas heated at 80°-100° C. for 2.5 h
  2. temperatureto cool
  3. filtrationfiltered
  4. extractionThe solid was thoroughly extracted with Et2O
  5. dry with materialthe extract was dried (Na2SO4)
  6. additiontreated with carbon
  7. concentrationconcentrated to an oil
  8. extractionExtraction of the latter with pet ether
  9. temperaturecooling the extract