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ChemicalBook CAS DataBase List Methyl 6-(hydroxymethyl)nicotinate
56026-36-9

Methyl 6-(hydroxymethyl)nicotinate synthesis

5synthesis methods
-

Yield:56026-36-9 96%

Reaction Conditions:

Stage #1:dimethyl 2,5-pyridine dicarboxylate with calcium chloride in tetrahydrofuran;ethanol for 0.5 h;
Stage #2: with sodium tetrahydroborate;ethanol in tetrahydrofuran at 0;

Steps:

10.1
Step 1. Synthesis of methyl 6-(hydroxymethyl)nicotinate (55):A mixture of dimethyl pyridine-2,5-dicarboxylate (54; 100.0 g, 0.51 mol), CaCl2 (227.4 g, 2.05 mol), THF (1100 mL) and EtOH (1200 mL) was stirred for 30 min, NaBH4 (48.6 g, 1.28 mol) was added portionwise at 0oC. The mixture was stirred for 18 hours. Saturated NH4Cl solution (1.5 L) and water (2.0L) was added slowly, and the resulting mixture was extracted with dichloromethane (3 x 3.0 L). The combined organic solvent was dried over MgSO4 and concentrated to give methyl 6- (hydroxymethyl)nicotinate 55 (82.0 g, 96%).

References:

SIRTRIS PHARMACEUTICALS, INC.;NARAYAN, Radha;DISCH, Jeremy, S.;PERNI, Robert, B.;VU, Chi, B. WO2010/56549, 2010, A1 Location in patent:Page/Page column 103

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