HRID252984

反应详情

EQUATION

反应方程式

HRID 252984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

2-Methyl-4-chloro-6-morpholino-pyridine (50 mmol) is dissolved in tetrahydrofuran (200 mL). The reaction is chilled to −78° C. under an inert atmosphere. A solution of n-butyllithium in hexanes (24 mL, 2.5M, 60 mmol) is added, and the reaction mixture is stirred for thirty minutes. A solution of oxirane dissolved in tetrahydrofuran (40 mL, 41.5M, 60 mmol) is added, and the reaction is allowed to warm to room temperature while stirring overnight. The solvent is removed under reduced pressure, and the crude material is dissolved in methylene chloride (200 mL) and washed with saturated ammonium chloride (2×50 mL), dried with sodium sulfate, and evaporated to dryness. The compound is purified by column chromatography to give 3-(4-chloro-6-morpholin-4-yl-pyrid-2-yl)-propan-1-ol.

WORKUP

后处理

  1. additionis added
  2. temperatureto warm to room temperature
  3. stirringwhile stirring overnight
  4. customThe solvent is removed under reduced pressure
  5. dissolutionthe crude material is dissolved in methylene chloride (200 mL)
  6. washwashed with saturated ammonium chloride (2×50 mL)
  7. dry with materialdried with sodium sulfate
  8. customevaporated to dryness
  9. customThe compound is purified by column chromatography