HRID1721178

反应详情

EQUATION

反应方程式

HRID 1721178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(7-bromo-2-quinolinylmethoxy)aniline: 0.32 g of NaH (95%) is added at 0° to a solution of 1.38 g of 3-aminophenol in 30 ml of DMF and then the batch is stirred for 30 min. at 0°. 3.2 g of 2-chloromethyl-7-bromo-quinoline in solid form are then added thereto and the batch is stirred for a further one hour at 0° and for another hour at 20°. It is then diluted with ethyl acetate, washed with water, dried over Na2SO4 and concentrated by evaporation. The evaporation residue is chromatographed on 250 g of silica gel. The product-containing fractions eluted with toluene/ethyl acetate 95:5 are combined and concentrated by evaporation to give the title compound which is further purified by crystallisation from CH2Cl2 /ether/hexane.

WORKUP

后处理

  1. stirringthe batch is stirred for a further one hour at 0° and for another hour at 20°
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated by evaporation
  5. customThe evaporation residue is chromatographed on 250 g of silica gel
  6. washThe product-containing fractions eluted with toluene/ethyl acetate 95:5
  7. concentrationconcentrated by evaporation