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ethyl (2E)-3-(5-chloropyridin-3-yl)prop-2-enoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
57%
NaH (570 mg, 14.24 mmol) was added portion wise to stirred anhydrous DMSO (10 ml_). The mixture was heated to 80C until evolution of gas ceased and then cooled to 0C. A solution of (carbethoxymethyl)- triphenylphosphonium bromide (3.05 g, 7.12 mmol) in DMSO (10 ml_) was then added and the mixture stirred at r.t for 30 min. The mixture was cooled to 0C and a solution of <strong>[113118-82-4]5-chloronicotinaldehyde</strong> (1 .0 g, 7.12 mmol) in DMSO (10 ml_) was added and the mixture was stirred at r.t for 1 h. The mixture was then poured into aqueous 1 M HCI and extracted into DCM (3 x 50 ml_). The organics were combined and washed with H2O (3 x 100 ml_) and brine (3 x 100 ml_), separated, dried (MgSO ) and concentrated. Purification by flash silica column chromatography (gradient elution /'-hex to 25% EtOAc in /-hex) gave the title compound as a yellow solid (1 .1 g, 57%). LCMS (ES+) 271 (M+H)+.
ethyl (E)-3-(5-cyano-2-(pyrrolidin-1-yl)phenyl)acrylate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
81%
With sodium hydroxide; In water; for 8h;Inert atmosphere; Reflux; Green chemistry;
General procedure: To a 25 mL three-necked round-bottomed flask was added 4-fluoro-3-nitrobenzaldehyde (2b, 0.1691 g, 1.0 mmol), NaOH(0.0600 g, 1.5 mmol), (2-ethoxy-2-oxoethyl)triphenylphosphoniumbromide (4a, 0.6440 g, 1.5 mmol), piperidine (3b, 0.2968mL, 3.0 mmol), and H2O (5 mL), then heated to 50 °C. The reactionprogress was carefully monitored by TLC. After 10 min, thesolvent was evaporated under reduced pressure, and theresidue was purified by silica gel column chromatography.
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