Triphenylphosphine → HCID 68565032, Verbindung

HRID 1593546Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1593546
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[O:8][C:7]([CH3:14])([CH3:13])[CH:6]=[C:5]2[C:15]([F:18])([F:17])[F:16].O[CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:38]=[CH:37][C:27]([O:28][C:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:38]=[CH:37][C:27]([O:28][C:29]([CH3:36])([CH2:34][CH3:35])[C:30]([O:32][CH3:33])=[O:31])=[CH:26][CH:25]=1)[O:8][C:7]([CH3:14])([CH3:13])[CH:6]=[C:5]2[C:15]([F:16])([F:18])[F:17]

Komponenten

6

Edukt 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 665248776-Chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-olHCID 68565476HCID 68565476, Verbindung

Produkt 1

HCID 68565032HCID 68565032, VerbindungAusbeute 61,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 6-Chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-ol (0.66 g, 2.95 mmol), methyl 2-(4-(3-hydroxypropoxy)phenoxy)-2-methylbutanoate (1.0 g, 2.97 mmol) and triphenylphosphine (0.85 g, 3.24 mmol) in 25 mL THF is added diethyl azodicarboxylate (0.56 g, 3.21 mmol)(slight exotherm) and the reaction mixture is stirred at ambient temperature overnight (16 h). After concentrating under reduced pressure, the residue obtained is chromatographed over silica gel to provide methyl 2-(4-(3-((6-chloro-2,2-dimethyl-4-(trifluoromethyl)-2H-chromen-7-yl)oxy)propoxy)phenoxy)-2-methylbutanoate (0.99 g).

Aufarbeitung

  1. concentrationAfter concentrating under reduced pressure
  2. customthe residue obtained
  3. customis chromatographed over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-5d26e891d5f04f90b4e53f5c1d4be094
Quelldatensatz
uspto-grants-2007_11
Patentnummer
US07297715B2

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