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ChemicalBook CAS DataBase List 2-[2-(4-Fluorophenyl)-2-oxo-1-phenylethyl]-4-methyl-3-oxo-N-phenylpentanamide

2-[2-(4-Fluorophenyl)-2-oxo-1-phenylethyl]-4-methyl-3-oxo-N-phenylpentanamide synthesis

10synthesis methods
-

Yield:125971-96-2 73%

Reaction Conditions:

with potassium carbonate in isopropyl alcohol at 10 - 45;Product distribution / selectivity;

Steps:

1
Preparation of 4-fluoro-α-[2-methyl-1-oxopropyl]-γ-oxo-N-β-diphenylbenzenebutanamideEXAMPLE 1 The mixture containing 300 ml isopropanol and 100 g of the formula III is cooled to 10-15° C. Potassium carbonate 94 g is charged into the above contents keeping the temperature 10-15° C. A solution of 128 gm of formula II in 125 ml isopropanol is then added slowly in 2-3 hrs keeping temperature at 10-15° C. Temperature is allowed to reach at 25-30° C. Temperature is further raised to 40-45° C. and then maintained for 8-10 hrs with simultaneous monitoring on HPLC. After HPLC complies, isopropanol is removed under vacuum keeping temperature below 55° C. followed by the addition of 600 ml ethyl acetate at 40-45° C. 600 ml water is charged and the organic layer is collected. Solvent is removed under vacuum when a solid mass is seen. This solid is purified by using isopropanol and methanol. Purity 99.69% with 0.047% of DESFLUORO impurity, Difluoro almost nil and O-alkylated impurity to be 0.1% with yield of 73%.

References:

PAI, Ganesh Gurpur;KISHORE, K. Nanda;CHAUDHARI, Narendra P.;ANJANEYULU, N.;GHOGARE, B N. US2009/298907, 2009, A1 Location in patent:Page/Page column 6

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