1-Butanol → Bis(dibutylchlorotin) Phosphate

HRID 1106283Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1106283
[CH2:1]([Sn:5](Cl)([Cl:10])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].C(O)CCC.O.O.[P:19]([O-:23])([O-:22])([O-:21])=[O:20].[Na+].[Na+].[Na+]>O>[P:19]([OH:23])([O-:22])([O-:21])=[O:20].[CH2:1]([Sn+:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:10])[CH2:2][CH2:3][CH3:4].[CH2:1]([Sn+:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:10])[CH2:2][CH2:3][CH3:4]

Komponenten

5

Edukt 3

HCID 2631-ButanolHCID 12688Dibutyltin dichlorideHCID 18623014Trisodium;phosphate;dihydrate

Produkt 1

HCID 20553860Bis(dibutylchlorotin) Phosphate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A glass reactor was charged with 91.1 g (0.3 mole) dibutyltin dichloride, 200 cc n-butanol, 50 cc water and 27.3 g (0.15 mole) dibasic sodium phosphate dihydrate. The resultant mixture was heated under a nitrogen atmosphere and the water removed by azeotropic distillation until the vapor temperature reached 117° C. The reaction mixture was then filtered and the liquid phase was concentrated under reduced pressure. The liquid residue solidified upon standing and weighed 83 g. The product was found to contain 34.60% tin, 11.18% chlorine and 4.42% phosphorus. The calculated values for these elements in the expected product are 37.53% tin, 11.21% chlorine and 4.90% phosphorus.

Aufarbeitung

  1. customthe water removed by azeotropic distillation until the vapor temperature
  2. customreached 117° C
  3. filtrationThe reaction mixture was then filtered
  4. concentrationthe liquid phase was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7624373b99824b889b3cf0d978fd40db
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04312959

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