Bis(pyridine)iodonium tetrafluoroborate → Ethyl 2-(4-amino-2-chloro-5-iodophenoxy)-4-fluorobenzoate

HRID 573096

Reaktionsgleichung

Reaktionsgleichung von HRID 573096
[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:8]=2[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([Cl:21])[CH:3]=1.[B-](F)(F)(F)F.C1C=CN=CC=1.C1C=CN=CC=1.[IH2+:39]>ClCCl.C(OCC)(=O)C>[NH2:1][C:2]1[C:20]([I:39])=[CH:19][C:5]([O:6][C:7]2[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:8]=2[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([Cl:21])[CH:3]=1

Komponenten

5

Edukt 2

HCID 10883201Bis(pyridine)iodonium tetrafluoroborateHCID 67228057Ethyl 2-(4-amino-2-chlorophenoxy)-4-fluorobenzoate

Produkt 1

HCID 67228200Ethyl 2-(4-amino-2-chloro-5-iodophenoxy)-4-fluorobenzoate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of EXAMPLE 242A (8.15 g) in dichloromethane (60 mL) was added bis(pyridine)iodonium tetrafluoroborate (9.79 g). The mixture was stirred at room temperature for 4 hours. The mixture was diluted with ethyl acetate (200 mL) and washed with aqueous Na2S2O3, water, brine and dried over Na2SO4. The mixture was filtered, and the solvent was evaporated and the residue was loaded on a column and eluted with 10% ethyl acetate in hexane to give the pure product.

Aufarbeitung

  1. washwashed with aqueous Na2S2O3, water, brine
  2. dry with materialdried over Na2SO4
  3. filtrationThe mixture was filtered
  4. customthe solvent was evaporated
  5. washeluted with 10% ethyl acetate in hexane
  6. customto give the pure product

Quellen und Nachweise

ORD-Eintrag
ord-d2a86a0fd77946acac55dfc20a9409fe
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029404B2

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