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ChemicalBook CAS DataBase List Ilepcimide
82857-82-7

Ilepcimide synthesis

11synthesis methods
-

Yield:82857-82-7 87%

Reaction Conditions:

with polyethyleneimine supported triphenylphosphine in chloroform at 65;Inert atmosphere;Wittig Olefination;

Steps:

General Procedure for Wittig Reactions Using 8

General procedure: Polymer 8 (0.2 g, 0.4 mmol phosphine) was dissolved in CHCl3 (1 mL) in a 10-mL round-bottomed flask equipped with a magnetic stirrer and a reflux condenser, followed by 13a-b(0.3 mmol) and 16 (0.2 mmol). The mixture stirred at 65 C until the reaction was determined tobe complete by TLC or 1H NMR analysis. The reaction mixture was then cooled to rt and poured into a mixture of Et2O (10 mL) and hexane (30 mL) in a beaker. The flask was rinsed withadditional Et2O (10 mL), and the combined organic solution was allowed to stand for 10 minbefore it was filtered through a short pad of diatomaceous earth, using additional Et2O (2 x 10 mL)for rinsing. The filtrate was concentrated under reduced pressure to afford the desired product inan essentially pure state based on 1H NMR analysis

References:

Xia, Xuanshu;Toy, Patrick H. [Synlett,2015,vol. 26,# 12,art. no. ST-2015-W0209-L,p. 1737 - 1743] Location in patent:supporting information

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