HRID1048954

反应详情

EQUATION

反应方程式

HRID 1048954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 5-(2-hydroxypropan-2-yl)pyridine-3-carboxylate (0.179 g, 0.915 mmol) in methanol (4.57 mL) was added 1 N aqueous sodium hydroxide solution (2.74 mL, 2.74 mmol). The reaction was stirred at room temperature for 30 min and then concentrated under reduced pressure. The resulting residue was acidified via the addition of 1 N aqueous hydrogen chloride solution until the pH was 2. Ethyl acetate was then added, and the extracted organics were dried over magnesium sulfate, filtered and concentrated to provide the title compound: LCMS m/z 182.01 [M+H]+; 1H NMR (500 MHz, CD3OD) δ 8.91 (s, 1 H), 8.79 (d, J=1.8 Hz, 1 H), 8.43 (d, J=1.9 Hz, 1 H), 1.51 (s, 6 H).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionThe resulting residue was acidified via the addition of 1 N aqueous hydrogen chloride solution until the pH was 2
  3. additionEthyl acetate was then added
  4. dry with materialthe extracted organics were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated