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Diisopropylamine → Dichloro(diisopropylamino)borane

HRID 1595105
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1595105
[Cl:1][B:2]([Cl:4])Cl.[CH:5]([NH:8][CH:9]([CH3:11])[CH3:10])([CH3:7])[CH3:6].C(N(CC)CC)C>C(Cl)Cl>[CH:5]([N:8]([B:2]([Cl:4])[Cl:1])[CH:9]([CH3:11])[CH3:10])([CH3:7])[CH3:6]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7912DiisopropylamineHCID 8471TriethylamineHCID 25135Boron Trichloride

Produkt 1

HCID 4139105Dichloro(diisopropylamino)boraneAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a methylene chloride solution of trichloroborane (1.0 M, 100 ml, 0.10 mole) was added dropwise at −78° C. diisopropylamine (13.108 ml, 0.100 mole) over a 30 minute period. The solution was allowed to stir for 1 hour, during which a white precipitate formed. The mixture was allowed to warm to room temperature, and solvent was removed under reduced pressure. The residue was dissolved in 100 ml of dry toluene, triethylamine (13.94 ml, 0.10 mole) was added and the solution was stirred overnight at room temperature. The mixture was filtered, the residue was washed with 20 ml of toluene. Solvent was removed under reduced pressure from the combined filtrates, and the resulting oil was purified by vacuum distillation (25-28° C., 13 Pa, 0.1 mm) to give 9.2 g (51 percent) of product as a colorless liquid.

Aufarbeitung

  1. customformed
  2. customsolvent was removed under reduced pressure
  3. dissolutionThe residue was dissolved in 100 ml of dry toluene
  4. stirringthe solution was stirred overnight at room temperature
  5. filtrationThe mixture was filtered
  6. washthe residue was washed with 20 ml of toluene
  7. customSolvent was removed under reduced pressure from the combined filtrates
  8. distillationthe resulting oil was purified by vacuum distillation (25-28° C., 13 Pa, 0.1 mm)

Quellen und Nachweise

ORD-Eintrag
ord-7c389eb9f7f4450d9bc39e16b6c8e4a1
Quelldatensatz
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06284905B1

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