反应 #543608

反应方程式

EDC

3,3 diphenylpropionic acid

mono-boc piperizine

→

desired product

收率 76.0%

4-(3,3-diphenyl-propionyl)-piperazine-1-carboxylic acid tert-butyl ester

收率 76.0%

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) (200 ml)
3. 3
   洗涤The organic was washed with water (50 ml, 2×) and 10% NaOH (50 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 3,3 diphenylpropionic acid (1.45 g, 6.44 mmol) in dry CH2Cl2 (70 ml) was added mono-boc piperizine (1.32 g, 7.08 mmol) under nitrogen. To the reaction was added EDC (2.71 g, 14.16 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) (200 ml). The organic was washed with water (50 ml, 2×) and 10% NaOH (50 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using hexane:ethyl acetate (1:1) to give desired product in 76% yield.

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