Iodylbenzene → HCID 86655984, Verbindung

HRID 1188748Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1188748
CC1(C)OO1.[I:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].IC1C=CC([C:22]2[S:23][C:24]3[CH:30]=[C:29]([O:31][CH3:32])[CH:28]=[CH:27][C:25]=3[N:26]=2)=CC=1>ClCCl>[I:6]([C:9]1[CH:14]=[CH:13][C:12]([C:22]2[S:23][C:24]3[CH:30]=[C:29]([O:31][CH3:32])[CH:28]=[CH:27][C:25]=3[N:26]=2)=[CH:11][CH:10]=1)(=[O:8])=[O:7]

Komponenten

5

Edukt 3

HCID 101840IodylbenzeneHCID 115197DimethyldioxiraneHCID 67081740HCID 67081740, Verbindung

Produkt 1

HCID 86655984HCID 86655984, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A freshly prepared dimethyldioxirane solution (30 mL), as described above (para. [0035]) for the synthesis of simple iodylbenzene analogs, was added drop wise with stirring to an anhydrous dichloromethane (15 mL) solution of 4 (100 mg, 0.28 mmol) cooled in an ice bath. The resultant suspension was stirred at 0° C. for additional period of 2-3 hours and then at room temperature overnight. The yellow solid that was formed was collected by centrifugation and washed three times with dichloromethane. The residue was dried in vacuum to give 2-(4-iodylphenyl)-6-methoxy-1,3-benzothiazole (7) (95.4 mg, 84%) as a beige solid.

Aufarbeitung

  1. additionwas added drop wise
  2. temperaturecooled in an ice bath
  3. customat room temperature
  4. customovernight
  5. customThe yellow solid that was formed
  6. customwas collected by centrifugation
  7. washwashed three times with dichloromethane
  8. customThe residue was dried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ce54a8482a2046ae913743c35f2ead7a
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08674101B2

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