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

HRID 1579946ノート

反応式

HRID 1579946 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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)].

後処理

  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

出典と根拠

ORDレコード
ord-073edc8f41924737b6357787a100ba9b
出典データセット
uspto-grants-1976_01
特許番号
US03932390

反応ノート

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