ChemicalBook CAS DataBase List Brivaracetam Impurity 30

Brivaracetam Impurity 30 synthesis

11synthesis methods

Product Name:Brivaracetam Impurity 30
CAS Number:22530-99-0
Molecular formula:C8H14O2
Molecular Weight:142.2

69906-54-3
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22530-99-0
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Yield:22530-99-0 93%

Reaction Conditions:

with bis-trimethylsilanyl peroxide;1-hexyl-3-methylimidazolium chloroaluminate(III) at 0 - 20; for 3 h;Acidic conditions;Inert atmosphere;Baeyer-Villiger Ketone Oxidation;

Steps:

General procedure for cyclic ketones oxidation

General procedure: The ketone (1.5 mmol) and silyl peroxide (2.25 mmol for reactions with bis(silyl) peroxides and 3 mmol for reactions with t-butyl silyl peroxides) were added dropwise at 0 °C into the freshly synthesised [hmim][Al_xCl_y] (2 mmol for reactions with bis(silyl) peroxides and 3 mmol for reactions with t-butyl silyl peroxides). Next, the solution was stirred under a nitrogen atmosphere at room temperature for 1-24 h (depending on the reaction rate). After this time, 5 ml of water was added to the post-reaction mixture, and the water phase was extracted with methylene chloride or diethyl ether (10× 5 ml). The organic layer was washed with 5 ml of water, dried over anhydrous MgSO₄, filtered, concentrated in a vacuum (50 °C, 100 mbar) and purified by column chromatography (hexane:ethyl acetate (4:1)) when necessary. All products were characterised by comparison of their NMR spectra (see Supplementary data) with authentic samples [20].

References:

Baj, Stefan;S?upska, Roksana;Chrobok, Anna;Drozdz, Agnieszka [Journal of Molecular Catalysis A: Chemical,2013,vol. 376,p. 120 - 126]