Methane → 1-Hydroxy-3-(piperidin-2-yl)-propane-1,1-diphosphonic acid

HRID 1073735

반응식

HRID 1073735 반응식
Cl.[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][C:10]([OH:12])=O.N1C=CC=CC=1CCC(O)=O.[P:24]([OH:27])([OH:26])[OH:25].P(Cl)(Cl)Cl.C.[Na]>Cl.[Pt]=O.O>[OH:12][C:10]([P:24]([OH:27])(=[O:25])[OH:26])([P:24]([OH:27])(=[O:26])[OH:25])[CH2:9][CH2:8][CH:3]1[CH2:4][CH2:5][CH2:6][CH2:7][NH:2]1

참가 물질

10

반응물 6

HCID 297MethaneHCID 24387Phosphorus trichlorideHCID 107909Phosphorous acidHCID 5642923-(Pyridin-2-yl)propanoic acidHCID 5360545SodiumHCID 426143813-(Piperidin-2-yl)propanoic acid hydrochloride

생성물 1

HCID 142312031-Hydroxy-3-(piperidin-2-yl)-propane-1,1-diphosphonic acid

시약·촉매·용매 3

HCID 82844Platinum oxide (PtO)촉매HCID 313Hydrochloric Acid용매HCID 962Water용매2회

실험 절차

1.5 g. 3-(Piperidin-2-yl)-propionic acid hydrochloride (m.p.: 193°-195° C., prepared by hydrogenation of 3-(2-pyridyl)-propionic acid in hydrochloric acid medium in the presence of platinum oxide) and 1.3 g. phosphorous acid are melted together at 80° C. After allowing to cool, 1.4 ml. phosphorus trichloride is added dropwise and further heated for 20 hours to 90° C. After cooling, 20 ml. water are carefully added thereto and heated under reflux for 7 hours. The cooled solution is treated with charcoal, filtered and the filtrate evaporated. After drying, the residue is stirred up several times with acetone, then taken up in water, the solution brought with 2N aqueous sodium hydroxide solution to a pH ≈5 and mixed with methanol. After stirring for some time with ice cooling, the precipitate is filtered off with suction and dried. There is obtained 1.05 g. (37% of theory) of the monosodium salt x 2 mole water; m.p. 270°-274° C.; Mrel : 0.41.

후처리

  1. customare melted together at 80° C
  2. temperatureto cool
  3. temperaturefurther heated for 20 hours to 90° C
  4. temperatureAfter cooling
  5. temperatureheated
  6. temperatureunder reflux for 7 hours
  7. filtrationfiltered
  8. customthe filtrate evaporated
  9. customAfter drying
  10. additionmixed with methanol
  11. stirringAfter stirring for some time with ice cooling
  12. filtrationthe precipitate is filtered off with suction
  13. customdried
  14. customThere is obtained 1.05 g

출처 및 근거

ORD 기록
ord-20598a6518244871bb008cfb204bdc1f
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971958

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