(2,6-Difluoro-3,5-dimethoxy-phenyl)-carbamic Acid Tert-Butyl Ester → 2,6-Difluoro-3,5-dimethoxybenzenamine

HRID 459945Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 459945
C(OC(=O)[NH:7][C:8]1[C:13]([F:14])=[C:12]([O:15][CH3:16])[CH:11]=[C:10]([O:17][CH3:18])[C:9]=1[F:19])(C)(C)C>FC(F)(F)C(O)=O>[F:14][C:13]1[C:12]([O:15][CH3:16])=[CH:11][C:10]([O:17][CH3:18])=[C:9]([F:19])[C:8]=1[NH2:7]

Komponenten

3

Edukt 1

HCID 86590945(2,6-Difluoro-3,5-dimethoxy-phenyl)-carbamic Acid Tert-Butyl Ester

Produkt 1

HCID 102618922,6-Difluoro-3,5-dimethoxybenzenamineAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

To 34.6 g (0.12 mol) of (2,6-difluoro-3,5-dimethoxy-phenyl)-carbamic acid tert-butyl ester, 120 mL of trifluoroacetic acid was added to give a homogeneous solution which was stirred at room temperature for 30 minutes. After 30 min., the reaction mixture was concentrated in vacuo. To the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8. The resulting suspension was extracted twice with diethylether. Combined diethylether layers were washed once with brine, dried over sodium sulfate, filtered and evaporated to give 22 g (97%) of title compound. MS (APCI) (m+1)/z 190.1.

Aufarbeitung

  1. customto give a homogeneous solution which
  2. waitAfter 30 min.
  3. concentrationthe reaction mixture was concentrated in vacuo
  4. additionTo the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8
  5. extractionThe resulting suspension was extracted twice with diethylether
  6. washCombined diethylether layers were washed once with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f425581ce63947c2a19ca9b8f355ec1f
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07196090B2

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