Penehyclidine Impurity 18 synthesis
- Product Name:Penehyclidine Impurity 18
- CAS Number:63624-23-7
- Molecular formula:C21H25NO2
- Molecular Weight:323.43
Yield:63624-23-7 75.2%
Reaction Conditions:
Stage #1: 3-quinuclidinolwith sodium hydride in dimethyl sulfoxide at 60; for 1 h;
Stage #2: 1,1-diphenyloxirane in dimethyl sulfoxide at 60; for 4 h;
Steps:
1 Preparation of 2-(3-quinuclidinyloxy)-1,1-diphenylethanol
12.71g (0.1mol) 3-quinuclidinol was added to a 500ml three-necked flask, added with 100ml of DMSO, stirred and dissolved, slowly added 4.2g (0.105mol) of 60% sodium hydride, heated to 60 °C, stirred 1 In an hour, 21.56 g (0.11 mol) of 2,2-diphenylethylene oxide in 80 mL of DMSO was added thereto, and the reaction was further stirred at this temperature for 4 hours, and the temperature was lowered to 10 °C. Add 150 ml of water, extract the organic phase three times with methyl tert-butyl ether,Dry over anhydrous sodium sulfate and concentrate to dryness under reduced pressure. A pale yellow viscous oil of 24.3 g was obtained in a yield of 75.2%.
References:
CN109824662,2019,A Location in patent:Paragraph 0024-0026
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