HRID411867

反应详情

EQUATION

反应方程式

HRID 411867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-(p-Toluenesulfonylmethyl)-2,6-dihydroxymethyl-s-triazine is dissolved in DMF and sodium azide (1.1 eq.) is added. The reaction mixture is heated to 50° C. for 4 hours. The DMF is removed under reduced pressure and the residue is partitioned between CH2Cl2 and water. The CH2Cl2 layer is separated and the water layer is extracted several times with CH2Cl2. The CH2Cl2 layers are combined, dried (MgSO4), and concentrated. The resultant residue is purified by silica gel flash column chromatography to give 4-(azidomethyl)-2,6-dihydroxymethyl-s-triazine.

WORKUP

后处理

  1. customThe DMF is removed under reduced pressure
  2. customthe residue is partitioned between CH2Cl2 and water
  3. customThe CH2Cl2 layer is separated
  4. extractionthe water layer is extracted several times with CH2Cl2
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe resultant residue is purified by silica gel flash column chromatography