HRID2173317

反应详情

EQUATION

反应方程式

HRID 2173317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of ethyl [6-(1H-tetrazol-1-yl)pyridin-3-yl]acetate (30.0 g, 129 mmol) in 150 mL of water was added 28 mL of 5M aq NaOH (141 mmol) over 5 min while cooled in a water bath. A very mild exotherm to +22° C. was observed. The mixture was stirred for 40 min at rt whereupon 106 mL of 2M aq H3PO4 was added over 30 min at rt. The resulting suspension was filtered, and the filter cake was washed with 2×50 mL water and dried on the frit under a stream of nitrogen overnight to afford [6-(1H-tetrazol-1-yl)pyridin-3-yl]acetic acid. This material was identical by H NMR to that synthesized according to method 1 above.

WORKUP

后处理

  1. temperaturewhile cooled in a water bath
  2. customto +22° C.
  3. additionwas added over 30 min at rt
  4. filtrationThe resulting suspension was filtered
  5. washthe filter cake was washed with 2×50 mL water
  6. customdried on the frit under a stream of nitrogen overnight