HRID495887
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe DMF is removed under reduced pressure
- customthe residue is partitioned between CH2Cl2 and water
- customThe CH2Cl2 layer is separated
- extractionthe water layer is extracted several times with CH2Cl2
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe resultant residue is purified by silica gel flash column chromatography