Triphenylphosphine → HCID 88049744, Verbindung

HRID 1882749Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1882749
CCOC(/N=N/C(OCC)=O)=O.[F:13][C:14]([F:43])([C:33]([F:42])([F:41])[C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])[CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:21]=[N:22][C:23]([C:26]2[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=2)=[N:24][CH:25]=1.[CH2:44](O)[CH2:45][CH2:46][CH2:47]/[CH:48]=[CH:49]\[CH2:50][CH3:51].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[F:43][C:14]([F:13])([C:33]([F:41])([F:42])[C:34]([F:39])([F:40])[C:35]([F:36])([F:37])[F:38])[CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:25]=[N:24][C:23]([C:26]2[CH:27]=[CH:28][C:29]([O:32][CH2:51][CH2:50][CH2:49][CH2:48]/[CH:47]=[CH:46]\[CH2:45][CH3:44])=[CH:30][CH:31]=2)=[N:22][CH:21]=1

Komponenten

6

Edukt 4

HCID 11776TriphenylphosphineHCID 5352837(Z)-5-Octen-1-olHCID 5462977Diethyl azodicarboxylateHCID 1355858974-[5-(5,5,6,6,7,7,8,8,8-Nonafluorooctyloxy)-pyrimidin-2-yl]-phenol

Produkt 1

HCID 88049744HCID 88049744, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of DEAD (0.261 g, 1.50 mmol) in THF (20 ml) was added dropwise to a stirred solution of 4-[5-(5,5,6,6,7,7,8,8,8-nonafluorooctyloxy)-pyrimidin-2-yl]-phenol (0.858 g, 1.50 mmol), cis-5-octene-1-ol (0.192 g, 1.50 mmol) and triphenylphosphine (0.939 g, 1.50 mmol) in THF (30 ml) and the reaction mixture stirred at room temperature for 24 h. The solvent was removed in vacuo and the residues purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (4:1)] to yield a colorless solid, which was recrystallized from ethanol.

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customthe residues purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (4:1)]
  3. customto yield a colorless solid, which
  4. customwas recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-bac502f1ac3843a9b9f445ff9081f9fe
Quelldatensatz
uspto-grants-2004_07
Patentnummer
US06759101B2

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