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
PROCEDURE
实验过程
A solution of ammonia may be used in place of hexamethylenetetramine to prepare 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide. Tris(hydroxymethyl)phosphine (3.9 g, 80%, 0.025 moles) was dissolved in formalin (20 ml, 40%, 0.267 moles) and water (20 ml). Ammonium hydroxide (29% NH3, 1.7 ml, 0.025 moles) was added to the solution at room temperature. Sulfamide (2.4 g, 0.025 mole) was then added and dissolved in the solution at room temperature. The solution heated up slightly and over the next twenty-four hours a precipitate formed. Filtration, dissolution of the solid in 4 successive 30 ml acetone washes and evaporation of the acetone yielded 1.0 g of crude 2-thia-1,3,5-triaza-7-phosphaadamantane (19.3% yield).
WORKUP
后处理
- dissolutiondissolved in the solution at room temperature
- temperatureThe solution heated up slightly and over the next twenty-four hours a precipitate
- customformed
- filtrationFiltration, dissolution of the solid
- customin 4 successive 30 ml acetone washes and evaporation of the acetone