Pyridine → Tris-(tributylammonium) pyrophosphate

HRID 1729130

Reaktionsgleichung

Reaktionsgleichung von HRID 1729130
O.O.O.O.O.O.O.O.O.O.[O-:11][P:12]([O:15][P:16]([O-:19])([O-:18])=[O:17])(=[O:14])[O-:13].[Na+].[Na+].[Na+].[Na+].[CH2:24]([N:28]([CH2:33][CH2:34][CH2:35][CH3:36])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH3:27].N1C=CC=CC=1>O.CN(C)C=O>[O-:13][P:12]([O:15][P:16]([OH:19])([O-:18])=[O:17])(=[O:11])[O-:14].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36].[CH2:33]([NH+:28]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:29][CH2:30][CH2:31][CH3:32])[CH2:34][CH2:35][CH3:36]

Komponenten

6

Edukt 3

HCID 1049PyridineHCID 7622TributylamineHCID 3084150Sodium pyrophosphate decahydrate

Produkt 1

HCID 22621555Tris-(tributylammonium) pyrophosphate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

Tetrasodium pyrophosphate decahydrate (4.46 g, 10 mmol) was dissolved in the minimum amount of water (about 50 mL) and passed through a column of AG50W X8 resin (100-200 mesh, 4×10 cm bed) poured in water. The column was eluted with water and the eluent was collected in an ice-cooled flask until pH of the eluent approached neutrality. Tri-n-butylamine (Aldrich Gold Label, 7.1 mL, 30 mmol) was added to the eluent and the two phases were stirred vigorously until all of the amine dissolved. The resulting solution was lyophilized. The residue was co-evaporated twice with dry pyridine and once with dry dimethylformamide. The residue was dissolved in dry dimethylforamide (10 mL) and the resulting 1.0 M solution was stored (for as long as one month) at 0° under argon until used.

Aufarbeitung

  1. washThe column was eluted with water
  2. customthe eluent was collected in an ice-
  3. temperaturecooled flask until pH of the eluent
  4. dissolutiondissolved
  5. custom(for as long as one month)
  6. customat 0°

Quellen und Nachweise

ORD-Eintrag
ord-61d6f0138b9542268b1cc597b3e8f6ae
Quelldatensatz
uspto-grants-1994_07
Patentnummer
US05332666

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