Hydrochloric Acid → HCID 59202372, Verbindung

HRID 1967653Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1967653
[CH3:1][N:2]([CH3:33])[C:3]1[CH:29]=[CH:28][C:6]([C:7]([NH:9][C:10]2[C:15]([CH3:16])=[CH:14][C:13]([C:17]([F:26])([C:22]([F:25])([F:24])[F:23])[C:18]([F:21])([F:20])[F:19])=[CH:12][C:11]=2[CH3:27])=[O:8])=[CH:5][C:4]=1[N+:30]([O-])=O.[Sn](Cl)(Cl)(Cl)Cl.Cl>C(O)(C)C>[NH2:30][C:4]1[CH:5]=[C:6]([CH:28]=[CH:29][C:3]=1[N:2]([CH3:33])[CH3:1])[C:7]([NH:9][C:10]1[C:15]([CH3:16])=[CH:14][C:13]([C:17]([F:26])([C:22]([F:23])([F:24])[F:25])[C:18]([F:20])([F:21])[F:19])=[CH:12][C:11]=1[CH3:27])=[O:8]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 24287Tin tetrachlorideHCID 59202384HCID 59202384, Verbindung

Produkt 1

HCID 59202372HCID 59202372, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

4-Dimethylamino-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-3-nitrobenzamide (3.0 g, 6.2 mmol) (see Example I6) was dissolved in isopropanol (50 ml) and tin chloride (4.2 g, 22.3 mmol) was added. The mixture was cooled to 0° C. and a solution of concentrated hydrogen chloride (6 ml) was added slowly. The reaction mixture was stirred at 80° C. for 2 hours. Then ⅓ of the total volume of isopropanol was evaporated. Water (100 ml) was added to the concentrated mixture and a solution of aqueous sodium hydroxide (4N) to adjust the pH to 7-8. The aqueous phase was extracted three times with ethyl acetate (200 ml). The combined organic extracts were dried over sodium sulfate and concentrated. The residue was used without further purification (2.7 g, 96% yield).

Aufarbeitung

  1. customThen ⅓ of the total volume of isopropanol was evaporated
  2. additionWater (100 ml) was added to the concentrated mixture
  3. extractionThe aqueous phase was extracted three times with ethyl acetate (200 ml)
  4. dry with materialThe combined organic extracts were dried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was used without further purification (2.7 g, 96% yield)

Quellen und Nachweise

ORD-Eintrag
ord-25e679af56bc4e7bbece37192066bc35
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08420855B2

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