HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 2-Thia-1,3,5-triaza-7-phosphaadamantane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Hexamethylenetetramine | HCID 4101 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Tris(Hydroxymethyl)Phosphine | HCID 76001 | — |
| Reactant | Sulfamide | HCID 82267 | — |
| Reactant | 2-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide | HCID 21829293 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Thia-1,3,5-triaza-7-phosphaadamantane | HCID 20360148 | 19.3% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03932390 |
| Source dataset | uspto-grants-1976_01 |
| ORD ID | ord-44977e02f2654b01bd686bd838993b62 |
| Source note | uspto-grants-1976_01 |