Phosphoric Acid → Phosphate

HRID 1290033Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1290033
Cl.N1(CCOC2C=CC(C(O)=O)=CC=2)CCCCC1.[CH2:20]([S:28]([O-:31])(=[O:30])=[O:29])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].[Na+].[P:33](=[O:37])([OH:36])([OH:35])[OH:34].[OH-].[Na+]>O.C(#N)C>[P:33]([O-:37])([O-:36])([O-:35])=[O:34].[CH2:20]([S:28]([O-:31])(=[O:29])=[O:30])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]

Komponenten

8

Edukt 4

HCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 57438354-(2-Piperidinoethoxy)benzoic acid hydrochlorideHCID 23669624Sodium caprylyl sulfonate

Produkt 2

HCID 1061PhosphateHCID 35715191-Octanesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

HPLC analysis indicated substantially pure 4-(2-piperidinoethoxy)benzoic acid, hydrochloride with only minor amounts of the methyl ester. The HPLC analysis was conducted as follows: A Zorbax C8 column was used (length: 25 cm; diameter: 4.6 mm; particle size: 5 microns). A weak eluent (60 mM phosphate and 10 mM octane sulfonate) was prepared by combining 6.48 g sodium 1-octanesulfonate and 12 mL HPLC grade concentrated phosphoric acid. This mixture was diluted to 3 L with HPLC, water and the resulting solution was adjusted to pH 2 with sodium hydroxide. Acetonitrile was employed as a strong eluent. A solution of 60% weak eluent, 40% strong eluent was applied to the column at a flow rate of 1 mL/minute; detection -247 nm. Under the foregoing conditions, elution of the methyl ester occurred in five minutes; the unreacted acid eluted in 3.5 minutes.

Aufarbeitung

  1. washUnder the foregoing conditions, elution of the methyl ester
  2. washthe unreacted acid eluted in 3.5 minutes

Quellen und Nachweise

ORD-Eintrag
ord-2fc943528c904a5587dcb2da65f98278
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05750688

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