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With potassium tert-butylate; In DMF (N,N-dimethyl-formamide); at 0 - 20℃; for 3.5h;
To a slurry of potassium t-butoxid (46. 6 mmol, 5. 22 G, 1. 3 eq.) in anhydrous DMF (250 mL) cooled to 0 C was added methoxy dimethylmalonate (46. 6 MMOL, 7. 55 G, 1. 3 eq.) via syringe in small portions. The ENOLATE was allowed to form over approximately 30 minutes at which point 2-BROMO-5- (BROMOMETHYL) pyridine was added portionwise. The reaction mixture was allowed to warm slowly to room temperature over 3 hours. The reaction mixture was diluted with ethyl ether and transferred to a separator funnel containing saturated ammonium chloride. The layers were shaken and separated and the organic layer was washed with water. The organic layer was then dried over anhydrous magnesium sulfate and concentrated in vacuo. The yellow oil obtained was purified on a Biotage Sp4 65i over a gradient of 0-100 % ethyl acetate in hexanes to afford a colorless oil that solidified on standing (12. 1 g, quant.) LRMS : 333 (M+H) +. H NMR (DMSO-D6, 400 MHz) ; 8. 27 (1 H, s) 7. 45-7. 55 (2 H, m) 3. 82 (6 H, s) 3. 57 (3 H, s) 3. 42 (2 H, s)
To 17ml_ of a 30percent weight solution of sodium methoxide in methanol at O 0C was added 3.65 ml_ of dimethyl methoxymalonate and, in portions, 3.34 g of <strong>[57297-29-7]cyclopropanecarboxamidine hydrochloride</strong>. After 30 minutes the mixture was heated to reflux for 1.5 hours then cooled to room temperature. After 16 hours the mixture was cooled to O 0C and quenched with 8 ml_ of concentrated aq. HCI. The white precipitate was concentrated by vacuum filtration then dried in a vacuum oven at 50 0C overnight. 3.76g of P36 was obtained.
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