Flunarizine EP Impurity D synthesis
- Product Name:Flunarizine EP Impurity D
- CAS Number:693765-11-6
- Molecular formula:C26H26F2N2
- Molecular Weight:404.49
![1-Piperazineacetaldehyde, 4-[bis(4-fluorophenyl)methyl]-](/CAS/20210305/GIF/1522375-87-6.gif)
1522375-87-6
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Yield: 69.4% ， 9.3%
Reaction Conditions:
with potassium tert-butylate in dichloromethane at 5;Inert atmosphere;stereoselective reaction;Wittig Olefination;
Steps:
General Method for the Preparation of E/Z-1-Benzhydryl-4-cinnamylpiperazine Derivatives (5a-c)
General procedure: Benzyltriphenyl phosphonium chloride (17.9 mmol) (prepared according to thereported procedure [31]) was added to a solution of 4a-c (17.0 mmol) in dichloromethane (50 ml) under N2 atmosphere. The mixture was cooled to 5 °C and t-BuOK (41.3 mmol) was added under stirring. After completion, the reaction mixture was quenched into water (100 ml). The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated under vacuum to obtain crude material 5a-c. The crude was then subjected to column purification over SiO2 using EtOAc/hexane as an eluent to afford 1a-c[25] and 6a-c in pure form.
References:
Shivprakash;Reddy, G. Chandrasekara [Synthetic Communications,2014,vol. 44,# 5,p. 600 - 609] Location in patent:supporting information
![Piperazine, 1-[bis(4-fluorophenyl)methyl]-4-(2,2-dimethoxyethyl)-](/CAS/20210305/GIF/1522375-84-3.gif)