1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene → HCID 57541570, Verbindung

HRID 1522920Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1522920
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[NH2:15][C:16]1[CH:35]=[CH:34][C:19]([O:20][C:21]2[CH:26]=[CH:25][N:24]=[C:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:22]=2)=[CH:18][CH:17]=1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:10])[NH:15][C:16]2[CH:35]=[CH:34][C:19]([O:20][C:21]3[CH:26]=[CH:25][N:24]=[C:23]([C:27]([O:29][C:30]([CH3:31])([CH3:32])[CH3:33])=[O:28])[CH:22]=3)=[CH:18][CH:17]=2)=[CH:4][C:3]=1[C:11]([F:12])([F:13])[F:14]

Komponenten

4

Edukt 2

HCID 27332651-Chloro-4-isocyanato-2-(trifluoromethyl) benzeneHCID 57541500HCID 57541500, Verbindung

Produkt 1

HCID 57541570HCID 57541570, VerbindungAusbeute 98,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

At room temperature, 1-chloro-4-isocyanato-2-(trifluoromethyl)benzene (656 mg, 2.96 mmol, 1.05 eq) was dissolved in dichloromethane (5 mL). To the resulted solution, a solution of tert-butyl 4-(4-aminophenoxy)picolinate (805 mg, 2.81 mmol, 1 eq) in dichloromethane (5 mL) was slowly added dropwise. The mixture was stirred for 16 hours at room temperature. The solvent was removed under reduced pressure, and the resulted solid was purified by column chromatography (dichloromethane:methanol=30:1) to give the title compound (1.4 g, purity 95%, yield 85%) as a white solid.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. customthe resulted solid was purified by column chromatography (dichloromethane:methanol=30:1)

Quellen und Nachweise

ORD-Eintrag
ord-e2ff7a6926ce43afb2e22bad188d4f97
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09078933B2

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