Flurbiprofen Related Impurity 1 synthesis
- Product Name:Flurbiprofen Related Impurity 1
- CAS Number:42771-81-3
- Molecular formula:C20H21FO4
- Molecular Weight:344.38
Yield:42771-81-3 90%
Reaction Conditions:
with sodium nitrite;trichloroacetic acid;copper(I) chloride in benzene;
Steps:
7 Diethyl 2-methyl-2-(3'-fluoro-4'-phenyl)-phenyl-malonate
EXAMPLE 7 Diethyl 2-methyl-2-(3'-fluoro-4'-phenyl)-phenyl-malonate A mixture of diethyl 2-methyl-2-[(3'-fluoro-4'-amino)-phenyl]malonate (7.73 g; 0.0273 mole), trichloroacetic acid (5.5 g; 0.0336 mole), cuprous chloride (0.14 g; 0.0014 mole) and of trimethylorthoformate (6.8 g; 0.0637 mole) in benzene (140.6 g; 1.8 moles) was heated to 60° C. to the mixture aliquots of sodium nitrite (2.3 g; 0.033 mole) were added under stirring. The mixture was maintained under stirring for 43 hours at 60° C. and then hydrolyzed with water and diluted hydrochloric acid. The organic layer was separated, washed with water and concentrated. The residue was chromatographed on silica gel 60 (Merck 70-230 mesh) column eluding with 8:2 petroleum ether (40°-60° C.)/diethyl ether. 8.5 of diethyl 2-methyl-2-[(3'-fluoro-4'-phenyl)-phenyl]-malonate were obtained; m.p. 36°-38° C. Yield, 90%.
References:
US4542233,1985,A
78543-08-5
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42771-81-3
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110-46-3
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