Iodine → Butyl(iodo)diphenylstannane

HRID 505953

Reaktionsgleichung

Reaktionsgleichung von HRID 505953
[CH2:1]([Sn:5](C1C=CC=CC=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].[I:24]I>CO>[CH2:1]([Sn:5]([I:24])([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 2

HCID 807IodineHCID 298153Butyl(triphenyl)stannane

Produkt 1

HCID 68417447Butyl(iodo)diphenylstannane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel3×

Versuchsvorschrift

In a three-necked flask protected from light, butyltriphenyltin (21.05 g; 51.8 mmol) was dissolved in 50 mL of dry methanol. A solution of iodine (12.06 g; 47.5 mmol) in methanol was then added slowly. After stirring at room temperature during 16 hours, methanol was eliminated under vacuum. The residue was dissolved in petroleum ether and washed with a saturated aqueous solution of sodium thiosulphate. Organic layers were washed with a saturated NaCI solution and dried over MgSO4. Solvent was evaporated and the crude product was distilled using a Kugelrohr apparatus at 60° C. A colourless oil was obtained (22.2 g, 48.6 mmol).

Aufarbeitung

  1. washwashed with a saturated aqueous solution of sodium thiosulphate
  2. washOrganic layers were washed with a saturated NaCI solution
  3. dry with materialdried over MgSO4
  4. customSolvent was evaporated
  5. distillationthe crude product was distilled
  6. customat 60° C
  7. customA colourless oil was obtained (22.2 g, 48.6 mmol)

Quellen und Nachweise

ORD-Eintrag
ord-726b2b942a134ca4960de7ff4aff58ed
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07781610B2

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