Decafluorobiphenyl → HCID 10875244, Verbindung

HRID 382911

Reaktionsgleichung

Reaktionsgleichung von HRID 382911
[F:1][C:2]1[C:7]([C:8]2[C:13]([F:14])=[C:12]([F:15])[C:11](F)=[C:10]([F:17])[C:9]=2[F:18])=[C:6]([F:19])[C:5]([F:20])=[C:4]([F:21])[C:3]=1[F:22].[CH2:23]([O:30][C:31]([C:33]1[CH:39]=[CH:38][C:36]([O-:37])=[CH:35][CH:34]=1)=[O:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[K+].[K]>CN(C)C=O>[CH2:23]([O:30][C:31]([C:33]1[CH:34]=[CH:35][C:36]([O:37][C:11]2[C:10]([F:17])=[C:9]([F:18])[C:8]([C:7]3[C:2]([F:1])=[C:3]([F:22])[C:4]([F:21])=[C:5]([F:20])[C:6]=3[F:19])=[C:13]([F:14])[C:12]=2[F:15])=[CH:38][CH:39]=1)=[O:32])[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

Komponenten

5

Edukt 3

HCID 67949DecafluorobiphenylHCID 5462222PotassiumHCID 23672351HCID 23672351, Verbindung

Produkt 1

HCID 10875244HCID 10875244, VerbindungAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

37.4 g of decafluorobiphenyl (0.112 mol) are dissolved in 700 ml of dimethylformamide, the mixture is cooled to −10° C. using a cryostat, and a solution of 29.8 g of potassium 4-benzyloxycarbonylphenoxide (0.112mol) in 300 ml of dimethylformamide is then added dropwise over the course of 2 hours. After 48 hours at −10° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, the residue is taken up in a little tetrahydrofuran, and the solution is filtered through a silica-gel column. The clear solution obtained is evaporated in a rotary evaporator until a white solid precipitates out. The solid is then stirred in n-hexane, filtered off using a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 92%).

Aufarbeitung

  1. customThe dimethylformamide is then removed in a rotary evaporator
  2. filtrationthe solution is filtered through a silica-gel column
  3. customThe clear solution obtained
  4. customis evaporated in a rotary evaporator until a white solid
  5. customprecipitates out
  6. filtrationfiltered off
  7. filtrationa fluted filter
  8. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
  9. customdrying cabinet (yield: 92%)

Quellen und Nachweise

ORD-Eintrag
ord-5755cd6649ba4362b9da2de0783343fc
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06310238B1

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