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Phosphonic acid → Azacyclopentane-2,2-diphosphonic acid

HRID 267185
ノート
印刷プレビュー

反応式

HRID 267185 の反応式
[NH:1]1[CH2:5][CH2:4][CH2:3][C:2]1=O.[OH:7][PH:8]([OH:10])=[O:9].P(Cl)(Cl)Cl>O>[NH:1]1[CH2:5][CH2:4][CH2:3][C:2]1([P:8]([OH:10])(=[O:7])[OH:9])[P:8]([OH:10])(=[O:7])[OH:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 407Phosphonic acidHCID 120252-PyrrolidoneHCID 24387Phosphorus trichloride

生成物 1

HCID 12886166Azacyclopentane-2,2-diphosphonic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

85.0 gm of 2-pyrrolidone (1.0 mol) and 164 gm of H3PO3 (2.0 mols) were melted at 80°C. While stirring this melt, 176 ml of PCl3 (2.0 mols) were added thereto. The mixture was stirred for three additional hours and was left standing at 70°C overnight. Then, three liters of H2O were used for the hydrolysis. The solution was boiled with activated carbon; and after filtration, the reaction product was precipitated with acetone. The white substance was dissolved in water, and passed over a cation exchanger. The solution was concentrated; and the substance was separated upon the addition of ethanol. The yield of crystalline azacyclopentane-2,2-diphosphonic acid was 95 gm, or about 41% of the theory. The molecular weight of the compound was determined by titration to be 230 (calculated: 231.09).

後処理

  1. additionwere added
  2. waitwas left
  3. filtrationand after filtration
  4. customthe reaction product was precipitated with acetone
  5. dissolutionThe white substance was dissolved in water
  6. concentrationThe solution was concentrated
  7. customand the substance was separated upon the addition of ethanol

出典と根拠

ORDレコード
ord-c5f3f267239c41feab5f273d047f417b
出典データセット
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03941772

反応ノート

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