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4,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile → HCID 22013473, Verbindung

HRID 1005497
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1005497
[C:1]([CH2:14][CH2:15][C:16]#[N:17])([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]>C1COCC1>[F:2][C:1]([F:3])([C:4]([F:5])([F:6])[C:7]([F:8])([F:9])[C:10]([F:11])([F:12])[F:13])[CH2:14][CH2:15][CH2:16][NH2:17]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 145126814,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile

Produkt 1

HCID 22013473HCID 22013473, VerbindungAusbeute 13,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A 210-ml shaker tube was charged with 30 g of C4F9CH2CH2CN, 4.0 g of PtB on activated carbon (2%) and 30 ml THF. The vessel was closed, cooled, evacuated and pressured with hydrogen to 3.5 MPa. The vessel was heated to 110° C. and hydrogen pressure was adjusted to 10.3 MPa. The mixture was shaken for 16 h. The vessel was cooled and the gas was vented slowly. The contents were filtered and the filtrate was distilled to remove THF. The residue was distilled at reduced pressure to give 4,4,5,5,6,6,7,7,7-nonafluoroheptylamine (4.0 g, 13%, b.p. 94-97° C./24 kPa absolute) and di(4,4,5,5,6,6,7,7,7-nonailuoroheptyl)amine (20.5 g, 69%, b.p. 105-108° C./270 Pa absolute). The distillation residue (0.2 g) was mainly (C4F9CH2CH2CH2)3N.

Aufarbeitung

  1. customThe vessel was closed
  2. temperaturecooled
  3. customevacuated
  4. temperatureThe vessel was cooled
  5. filtrationThe contents were filtered
  6. distillationthe filtrate was distilled
  7. customto remove THF
  8. distillationThe residue was distilled at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-866895660b7147d3ad3492cec1773528
Quelldatensatz
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06054615

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