Phosphonic acid → Azacyclopentane-2,2-diphosphonic acid

HRID 267185

반응식

HRID 267185 반응식
[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]

참가 물질

5

반응물 3

HCID 407Phosphonic acidHCID 120252-PyrrolidoneHCID 24387Phosphorus trichloride

생성물 1

HCID 12886166Azacyclopentane-2,2-diphosphonic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c5f3f267239c41feab5f273d047f417b
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941772

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