反应详情

First, 7-methoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one (1.15 g, 6 mmol) is dissolved in absolute tetramethylurea (30 ml), mixed with 55% sodium hydride dispersion in oil (300 mg) and stirred for 2 hours at 20°-25° C. under a nitrogen atmosphere. The resulting reaction mixture is added dropwise, with stirring, at 15°-20° C. under a nitrogen atmosphere to 1-chloro-3-iodopropane (1.6 g, 7.8 mmol) dissolved in tetramethylurea (20 ml) and stirred for 3 hours at ambient temperature. Then, ethyl acetate (300 ml) are added and the mixture is extracted six times with water. The organic solution is dried over magnesium sulphate, concentrated by evaporation and the residue is purified oer a silica gel column with methylene chloride and increasing amounts of ethanol (up to 2%). Yield: 410 mg. IR spectrum (methylene chloride): 1650 cm-1 (C=O).

1. customThe resulting reaction mixture
2. additionis added dropwise
3. stirringstirred for 3 hours at ambient temperature
4. extractionthe mixture is extracted six times with water
5. dry with materialThe organic solution is dried over magnesium sulphate
6. concentrationconcentrated by evaporation
7. customthe residue is purified oer a silica gel column with methylene chloride
8. temperatureincreasing amounts of ethanol (up to 2%)