HRID275378
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
A solution of 6.8 g. of 4-acetyl-3-hydroxy-2propylbenzyl chloride and 14.9 g. of ethyl 4-aminobenzoate in 200 ml. of acetonitrile was heated to reflux for 48 hours. An additional 9.9 g. of ethyl 4aminobenzoate were added and the reaction was refluxed an additional 120 hours. The reaction mixture was cooled and concentrated in vacuo. The residue was dissolved in methylene chloride. The organic solution was washed first with a saturated sodium carbonate solution and then with water. The organic solution was then dried over sodium sulfate and evaporated to dryness. Chromatography of the residue afforded 7.4 g. of the desired title product. NMR.
WORKUP
后处理
- temperatureto reflux for 48 hours
- temperaturethe reaction was refluxed an additional 120 hours
- temperatureThe reaction mixture was cooled
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in methylene chloride
- washThe organic solution was washed first with a saturated sodium carbonate solution
- dry with materialThe organic solution was then dried over sodium sulfate
- customevaporated to dryness
- customChromatography of the residue afforded 7.4 g