1-(5-FLUORO-2-PYRIDINYL)-4-OXO-CYCLOHEXANECARBONITRILE synthesis
- Product Name:1-(5-FLUORO-2-PYRIDINYL)-4-OXO-CYCLOHEXANECARBONITRILE
- CAS Number:960371-10-2
- Molecular formula:C12H11FN2O
- Molecular Weight:218.23
960371-09-9
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960371-10-2
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Yield:-
Reaction Conditions:
with sodium chloride in water;dimethyl sulfoxide at 160; for 1 h;Heating / reflux;
Steps:
24.b
(b) To a solution of ketoester prepared above (3.6 g, 13 mmol) in DMSO (45 mL) containing boiling chips, was added NaCl (0.25 g, 4.3 mmol) and H2O (0.45 mL). The reaction was heated to 160° C. with a reflux condenser in place and stirred for 1 h. The reaction was diluted with H2O (10×) and extracted with Et2O (3×50 mL). The combined organic, were washed with brine, dried over MgSO4, and removed in vacuo. Silica gel chromatography (gradient elution 15-85% EtOAc in hexanes) afforded the ketone. 1H NMR (400 Hz, CDCl3): δ 2.4-2.65 (m, 6H), 2.80-2.89 (m, 2H), 7.45-7.51 (m, 1H), 7.70 (dd, J==12, 4 Hz, 1H), 8.46 (d, J=2.7 Hz, 1H).
References:
US2007/299080,2007,A1 Location in patent:Page/Page column 67-68
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960371-10-2
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