Ammonia → 2-Thia-1,3,5-triaza-7-phosphaadamantane

HRID 1579948노트

반응식

HRID 1579948 반응식
N.C1N2CN3CN(C2)CN1C3.[N:12]12[CH2:21][N:16]3[CH2:17][P:18]([CH2:20][N:14]([CH2:15]3)[S:13]1(=O)=O)[CH2:19]2.OCP(CO)CO.C=O.[OH-].[NH4+].S(N)(N)(=O)=O>O>[N:12]12[CH2:21][N:16]3[CH2:17][P:18]([CH2:20][N:14]([CH2:15]3)[S:13]1)[CH2:19]2

참가 물질

9

반응물 7

HCID 222AmmoniaHCID 712FormaldehydeHCID 4101HexamethylenetetramineHCID 14923Ammonium HydroxideHCID 76001Tris(Hydroxymethyl)PhosphineHCID 82267SulfamideHCID 218292932-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide

생성물 1

HCID 203601482-Thia-1,3,5-triaza-7-phosphaadamantane수율 19.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  1. dissolutiondissolved in the solution at room temperature
  2. temperatureThe solution heated up slightly and over the next twenty-four hours a precipitate
  3. customformed
  4. filtrationFiltration, dissolution of the solid
  5. customin 4 successive 30 ml acetone washes and evaporation of the acetone

출처 및 근거

ORD 기록
ord-44977e02f2654b01bd686bd838993b62
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03932390

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