反应详情

3.46 g (15 mmol) 11-chloro-6,11-dihydrodibenzo[b,e]oxepine are dissolved in 90 ml absolute dichloromethane and 5.43 g (15 mmol) N-(4-piperidin-4-yl-butyl)-3-pyridin-3-yl-propionamide dihydrochloride is added. 5.0 g (49.5 mmol) TEA is dissolved in 20 ml absolute dichloromethane and added dropwise under ice cooling. The mixture is stirred for two days at RT without further cooling. Subsequently, the batch is washed twice, each with 50 ml water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum. The resinous residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5) and after drawing off the solvent, is first crystallized twice, each from 10 ml 1-chlorobutane and subsequently once from 10 ml acetic acid ethyl ester. Colorless crystals with a MP of 110-112° C. in a yield of 0.2 g (3%) are recovered

1. additionadded dropwise under ice cooling
2. washSubsequently, the batch is washed twice
3. dry with materialThe organic phase is dried over sodium sulfate
4. customthe solvent is removed under vacuum
5. customThe resinous residue is chromatographically purified over silica gel with CHCl3/CH3OH (95/5)
6. customis first crystallized twice
7. customColorless crystals with a MP of 110-112° C. in a yield of 0.2 g (3%) are recovered