Trifluoroacetic acid → HCID 20314460, Verbindung

HRID 973311Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 973311
[S:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][C:16]([I:19](OC(=O)C)OC(=O)C)=[CH:15][CH:14]=2)=[CH:9][CH:8]=1.[F:28][C:29]([F:34])([F:33])[C:30]([OH:32])=[O:31]>C(OC(=O)C)(=O)C>[F:28][C:29]([F:34])([F:33])[C:30]([O-:32])=[O:31].[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:18]=[CH:17][C:16]([I+:19][C:2]3[S:1][CH:5]=[CH:4][CH:3]=3)=[CH:15][CH:14]=2)=[CH:11][CH:12]=1

Komponenten

5

Edukt 3

HCID 6422Trifluoroacetic acidHCID 8030ThiopheneHCID 20314474HCID 20314474, Verbindung

Produkt 1

HCID 20314460HCID 20314460, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7918Acetic AnhydrideLösungsmittel2×

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

A mixture of thiophene (8.7 g.) and acetic anhydride (60 ml.) is added to a stirred suspension of 4-(4-chlorophenyl)-(diacetoxyiodo)benzene (21.7 g.) in a mixture of acetic anhydride (50 ml.) and trifluoroacetic acid (15 ml.) below -10° C. during 1 hour. The mixture is stirred at -10° C. for 2 hours, at ambient temperature for 18 hours and is then filtered. The filtrate is concentrated to small volume in vacuo, and ether is added. The solid so formed is filtered off and crystallised from toluene to give 4-(4-chlorophenyl)-phenyl-2-thienyliodonium trifluoroacetate (13.7 g.), m.p. 175°-177° C.

Aufarbeitung

  1. filtrationis then filtered
  2. concentrationThe filtrate is concentrated to small volume in vacuo, and ether
  3. additionis added
  4. customThe solid so formed
  5. filtrationis filtered off
  6. customcrystallised from toluene

Quellen und Nachweise

ORD-Eintrag
ord-07508b027d284a738035660ac5d141f6
Quelldatensatz
uspto-grants-1977_10
Patentnummer
US04055595

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