Pyridine → Di-n-butyl 2-(di-n-butylmethylsily)-ethyl phosphate

HRID 2083178Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2083178
[CH2:1]([O:5][P:6](Cl)(=[O:12])[O:7][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:2][CH2:3][CH3:4].[CH2:14]([Si:18]([CH2:23][CH2:24][CH2:25][CH3:26])([CH3:22])[CH2:19][CH2:20][OH:21])[CH2:15][CH2:16][CH3:17].N1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[P:6]([O:21][CH2:20][CH2:19][Si:18]([CH2:14][CH2:15][CH2:16][CH3:17])([CH2:23][CH2:24][CH2:25][CH3:26])[CH3:22])([O:5][CH2:1][CH2:2][CH2:3][CH3:4])([O:7][CH2:8][CH2:9][CH2:10][CH3:11])=[O:12]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 94784Phosphorochloridic acid, dibutyl esterHCID 203579192-(Di-n-butyl methylsilyl)-ethanol

Produkt 1

HCID 20357920Di-n-butyl 2-(di-n-butylmethylsily)-ethyl phosphate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

Dibutylphosphorochloridate (3.74 g) was added to a solution of 2-(di-n-butyl methylsilyl)-ethanol (3 g) and pyridine (1.04 g) in carbon tetrachloride (10 ml). The mixture was left overnight, filtered, and the filtrate passed through an alumina column (20 g), eluting with a further 3 × 20 ml of carbon tetrachloride. Removal of the solvent under vacuum left the phosphate as a colourless oil (2.7 g).

Aufarbeitung

  1. filtrationfiltered
  2. washeluting with a further 3 × 20 ml of carbon tetrachloride
  3. customRemoval of the solvent under vacuum
  4. waitleft the phosphate as a colourless oil (2.7 g)

Quellen und Nachweise

ORD-Eintrag
ord-a6b6281a90494c5f910a1168acd55afd
Quelldatensatz
uspto-grants-1978_04
Patentnummer
US04084951

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