HRID1502158

反应详情

EQUATION

反应方程式

HRID 1502158 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium hydroxide (161 mg, 3.84 mmol) dissolved in water (3 mL) was added to ethyl 2-(5-(5-methyl-1H-tetrazol-1-yl)pyridin-2-yl)acetate (776 mg, 3.14 mmol) in THF (10 ml) and stirred at room temperature. The reaction was followed by TLC. Evaporated off the organics without heating and cooled in ice bath then acidified with 1N HCL (3.84 ml, pH ˜3). Extracted with EtOAc/THF (2×), washed with brine (1×), dried over Na2SO4, filtered and concentrated to yield 2-(5-(5-methyl-1H-tetrazol-1-yl)pyridin-2-yl)acetic acid: 1H-NMR (500 MHz, CD3OD) δ ppm 8.79 (d, J=2.4 Hz, 1H), 8.098 (dd, J=8.0, 2.5 Hz, 1H), 7.710 (d, J=8.3 Hz, 1H), 3.978 (s, 2H), 2.649 (s, 3H)

WORKUP

后处理

  1. customEvaporated off the organics
  2. temperaturewithout heating
  3. temperaturecooled in ice bath
  4. extractionExtracted with EtOAc/THF (2×)
  5. washwashed with brine (1×)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated