反应 #543612

反应方程式

EDC

1-(1-methyl-piperidin-4ylmethyl)-piperazine

3,3-diphenylpropanoic acid

→

desired product

收率 69.0%

1-[4-(1-methyl-piperidin-4-ylmethyl)piperazin-1-yl]-3,3-diphenyl-propan-1-one

收率 69.0%

溶剂

CH2Cl2

反应条件

后处理

1. 1
   浓缩The reaction was then concentrated under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue dissolved in ethyl acetate:water (10:1) (100 ml)
3. 3
   洗涤The organic was washed with water (25 ml, 2×) and 10% NaOH (25 ml)
4. 4
   干燥dried over MgSO4
5. 5
   其他evaporated to dryness
6. 6
   其他The resulting residue was purified by column chromatography

实验过程

To a solution of 1-(1-methyl-piperidin-4ylmethyl)-piperazine (0.25 g, 1.26 mmol) in dry CH2Cl2 (25 ml) was added 3,3-diphenylpropanoic acid (0.26 g, 1.15 mmol) under nitrogen. To the reaction was added EDC (0.48 g, 2.53 mmol) and DMAP (cat) and the reaction mixture stirred under nitrogen at room temperature overnight. The reaction was then concentrated under reduced pressure. The residue dissolved in ethyl acetate:water (10:1) (100 ml). The organic was washed with water (25 ml, 2×) and 10% NaOH (25 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using CH2Cl2:MeOH (5:1) to give desired product in 69% yield.

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