HRID2236540

反应详情

EQUATION

反应方程式

HRID 2236540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-azidomethyl-5-propoxy-pyridin-4-ol (9.70 g, 46.6 mole), is then suspended in 120 mL of tetrahydrofuran and treated with triphenylphosphine (12.22 g, 46.6 mmole) after stirring for 10 mins at ambient temperature water is added (12.6 mL, 15 equivalents) and the reaction mixture is stirred at ambient temperature overnight. The solids gradually dissolved followed by the formation of a precipitate. The resulting solid is filtered, washed with fresh 10:1 tetrahydrofuran:water and dried to give, 5.92 g, (69%), mp 159-60° C.; MS (ES+): m/z 183.3 (M+H).

WORKUP

后处理

  1. additionis added (12.6 mL, 15 equivalents)
  2. dissolutionThe solids gradually dissolved
  3. filtrationThe resulting solid is filtered
  4. washwashed with fresh 10:1 tetrahydrofuran
  5. dry with materialwater and dried
  6. customto give