[Cl:1][C:2]1[N:7]=[CH:6][C:5](CC#N)=[CH:4][CH:3]=1.Br[CH2:12][CH2:13]Cl.[OH-:15].[Na+].[CH2:17]([OH:20])[CH2:18]O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:18]2([C:17]([OH:20])=[O:15])[CH2:13][CH2:12]2)=[CH:4][CH:3]=1
To a stirred mixture of (6-chloropyridin-3-yl)acetonitrile (2.00 g, 0.0131 mol), benzyltriethylammonium chloride (0.2 g, 0.0008 mol), and 1-bromo-2-chloroethane (3.26 mL, 0.0393 mol), was added sodium hydroxide aqueous solution (50%, 3 mL, 0.08 mol) drop-wise at 50° C. The mixture was stirred at 50° C. for 5 h. 1,2-ethanediol (4 mL) was added to the above mixture and stirred at 100° C. overnight. The aqueous layer was acidified to pH ˜1, and extracted with ethyl acetate. The organic layer was washed with water and brine, dried with sodium sulfate, filtered, and concentrated to afford the desired compound (2.2 g, 85%). Analytical LCMS: (M+H)+=198.0.
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