Formaldehyde → 2-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide

HRID 1579946노트

반응식

HRID 1579946 반응식
O[CH2:2][P:3]([CH2:6]O)[CH2:4]O.C=O.[S:10]([NH2:14])([NH2:13])(=[O:12])=[O:11].[CH2:15]1N2CN3CN(C2)[CH2:17][N:16]1C3>O>[N:13]12[CH2:17][N:16]3[CH2:2][P:3]([CH2:6][N:14]([CH2:15]3)[S:10]1(=[O:12])=[O:11])[CH2:4]2

참가 물질

6

반응물 4

HCID 712FormaldehydeHCID 4101HexamethylenetetramineHCID 76001Tris(Hydroxymethyl)PhosphineHCID 82267Sulfamide

생성물 1

HCID 218292932-Thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide수율 66%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Tris(hydroxymethyl)phosphine (3.9 g, 80%, 0.025 moles) was dissolved in formalin (20 ml, 40%, 0.267 moles) and water (20 ml). Sulfamide (2.4 g, 0.025 mole) and hexamethylenetetramine (3.5 g, 0.025 mole) were added together 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 3.42 g of crude 2-thia-1,3,5-triaza-7-phosphaadamantane 2,2-dioxide (66% yield) [mp 274°-5° (water)].

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-073edc8f41924737b6357787a100ba9b
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03932390

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