3-Iodophthalic anhydride → 6-iodo-N-{2-methyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]phenyl}phthalamic acid

HRID 1373506

Reaktionsgleichung

Reaktionsgleichung von HRID 1373506
[I:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:4]2[C:5]([O:7][C:8](=[O:9])[C:3]=12)=[O:6].[CH3:13][C:14]1[CH:20]=[C:19]([C:21]([F:30])([C:26]([F:29])([F:28])[F:27])[C:22]([F:25])([F:24])[F:23])[CH:18]=[CH:17][C:15]=1[NH2:16]>C(#N)C>[I:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:4]([C:5]([NH:16][C:15]2[CH:17]=[CH:18][C:19]([C:21]([F:30])([C:22]([F:23])([F:24])[F:25])[C:26]([F:27])([F:28])[F:29])=[CH:20][C:14]=2[CH3:13])=[O:6])[C:3]=1[C:8]([OH:7])=[O:9]

Komponenten

4

Edukt 2

HCID 2820713-Iodophthalic anhydrideHCID 99255434-(1,1,1,2,3,3,3-Heptafluoropropan-2-yl)-2-methylaniline

Produkt 1

HCID 120543996-iodo-N-{2-methyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]phenyl}phthalamic acidAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

In acetonitrile (100 ml) was dissolved 5.5 g (20 mmol) of 3-iodophthalic anhydride, and a solution (20 ml) of 5.5 g (20 mmol) of 2-methyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]aniline in acetonitrile was slowly dropped thereinto. After the resulting mixture was stirred at room temperature for 3 hours, two-thirds of the acetonitrile was distilled off under reduced pressure and the crystals precipitated were filtered and then washed with acetonitrile to obtain 5.6 g (yield 51%) of 6-iodo-N-{2-methyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]phenyl}phthalamic acid.

Aufarbeitung

  1. distillationtwo-thirds of the acetonitrile was distilled off under reduced pressure
  2. customthe crystals precipitated
  3. filtrationwere filtered
  4. washwashed with acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-8c41ddaf55364930abd2412d765a58e9
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07161032B2

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