Hydrochloric Acid → Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene

HRID 2092686

Reaktionsgleichung

Reaktionsgleichung von HRID 2092686
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[F:11][C:12]([F:17])([F:16])[CH:13]([OH:15])[CH3:14].C(=O)([O-])[O-].[Cs+].[Cs+].Cl>CC#N.O.C(OCC)(=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([O:15][CH:13]([CH3:14])[C:12]([F:17])([F:16])[F:11])=[CH:3][CH:4]=1)([O-:10])=[O:9]

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 9590p-FluoronitrobenzeneHCID 97741,1,1-Trifluoro-2-propanolHCID 10796Cesium carbonate

Produkt 1

HCID 66577895Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of 1-fluoro-4-nitrobenzene (4.24 g, CAS Reg. No. 350-46-9), 1,1,1-trifluoro-propan-2-ol (4.56 g, CAS Reg. No. 374-01-6) and cesium carbonate (13.04 g) in CH3CN (50 mL) was heated to reflux for 10 hours. Then, the reaction mixture was cooled, acidified with conc. HCl and then distributed between ethyl acetate and water. The organic layer was separated, washed with brine and evaporated to provide the title compound (6.74 g) that was used without further purification. Rf: 0.38 (silica gel, ether/heptane 1:4).

Aufarbeitung

  1. temperatureto reflux for 10 hours
  2. temperatureThen, the reaction mixture was cooled
  3. customThe organic layer was separated
  4. washwashed with brine
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-7192b305e37e41689e71164ccf5399fb
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08440710B2

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