HRID626186

反应详情

EQUATION

反应方程式

HRID 626186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of methyl 1-methyl-2-oxo-1,2-dihydropyridine-4-carboxylate (1 g, 1.0 eq) in 25 mL MeOH was added a solution of LiOHH2O (755 mg, 3.0 eq) in 5 mL water at rt. The reaction was then stirred at rt for 2 h. Then the solvent was removed in vacuo, and water was added to the residue, followed by addition of 3N HCl (aq) to adjust pH=1˜3. The product was collected by filtration and washed with water to give the product as white solid (540 mg, 60% yield). 1H NMR (400 MHz, DMSO-d6) δ 13.56 (brs, 1H), 7.80 (d, J=7.2 Hz, 1H), 6.83 (d, J=1.6 Hz, 1H), 6.53 (d, J=6.8 Hz, 1.6 Hz, 1H), 3.46 (s, 3H).

WORKUP

后处理

  1. customThen the solvent was removed in vacuo, and water
  2. additionwas added to the residue
  3. additionfollowed by addition of 3N HCl (aq)
  4. filtrationThe product was collected by filtration
  5. washwashed with water