Choline Fenofibrate Impurity 1 synthesis
- Product Name:Choline Fenofibrate Impurity 1
- CAS Number:2985-79-7
- Molecular formula:C13H9ClO2
- Molecular Weight:232.66
? with aluminium chloride without solvent between 120° and 160°, (29%), at 200° for 20 min or in refluxing chlorobenzene for 10 h (53%);
? with trifluoromethanesulfonic acid at 45–55° (6%).
Yield:2985-79-7 98%
Reaction Conditions:
with dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer;copper diacetate in N,N-dimethyl-formamide at 80; for 8 h;Sealed tube;
Steps:
General procedure: A mixture of salicylaldehyde (0.2 mmol) and arylboronic acid (0.4 mmol) was dissolved in DMF (2 mL) and [Cp*RhCl2]2 (4.9 mg,4 mol %) and Cu(OAc)2 (72.8 mg, 0.4 mmol) was added. Then the reaction was conducted in a sealed tube at a temperature of 80 C for 8 h. The reaction mixture was diluted with ethylacetate (20 mL),washed with H2O (310 mL). The organic layer was then dried over anhydrous Na2SO4, filtered and concentrate. The crude product was loaded on a silica gel column and flashed with 5-10% ethyl acetate in petroleum ether to afford the desired products 3 as solid or liquid
References:
Wang, Dahai;Cui, Sunliang [Tetrahedron,2015,vol. 71,# 45,p. 8511 - 8516]
1195709-59-1
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