HRID1721181
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-(7-acetyl-2-quinolinylmethoxy)aniline: 30 mg of NaH (95%) are added at 0° to a solution of 0.13 g of 3-aminophenol in 2.5 ml of DMF and then the batch is stirred for 30 min. at 0°. 0.25 g of 2-chloromethyl-7-acetyl-quinoline in solid form is then added 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 25 g of silica gel. The product-containing fractions eluted with toluene/ethyl acetate 85:15 are combined and concentrated by evaporation to give the title compound which is further reacted directly.
WORKUP
后处理
- stirringthe batch is stirred for a further one hour at 0° and for another hour at 20°
- washwashed with water
- dry with materialdried over Na2SO4
- concentrationconcentrated by evaporation
- customThe evaporation residue is chromatographed on 25 g of silica gel
- washThe product-containing fractions eluted with toluene/ethyl acetate 85:15
- concentrationconcentrated by evaporation