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

HRID 1073735

反应方程式

HRID 1073735 反应方程式
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

参与物

10

反应物 6

HCID 297天然气HCID 24387三氯化磷HCID 107909正亚磷酸HCID 5642923-吡啶-2-基-丙酸HCID 5360545钠HCID 426143812-Piperidinepropanoic acid, hydrochloride

产物 1

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

试剂、催化剂与溶剂 3

HCID 82844Platinum oxide (PtO)催化剂HCID 313海萝胶溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-20598a6518244871bb008cfb204bdc1f
来源数据集
uspto-grants-1990_11
专利号
US04971958

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