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Hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium;pyridine → HCID 57097671, Verbindung

HRID 2211329
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2211329
[CH3:1][C@@:2]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][CH:3]2[OH:9].[Cr](O[Cr](O)(=O)=O)(O)(=O)=O.N1C=CC=CC=1>C(Cl)Cl.C(OCC)C>[CH3:1][C@@:2]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][C:3]2=[O:9]
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Komponenten

5

Edukt 2

HCID 18757208Hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium;pyridineHCID 57313420HCID 57313420, Verbindung

Produkt 1

HCID 57097671HCID 57097671, VerbindungAusbeute 64,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

79.6 g (0.63M) of the optically active alcohol (V) obtained in 1-4) above was dissolved in 300 ml of methylene chloride and the resulting solution was added dropwise to a suspension of 304 g (0.81M) of pyridine dichromate in 700 ml of methylene chloride at room temperature. Then the resulting mixture was stirred for three days. The obtained reaction mixture was diluted with 1 l of diethyl ether and filtered through celite. The filtrate was dried over anhydrous magnesium sulfate and the solvent was evaporated. The residue was distilled under reduced pressure to give 50.4 g (theoretical yield: 64.5%) of the aimed compound (VI) as a colorless oily material. b.p.: 70° C./20 mmHg.

Aufarbeitung

  1. customThe obtained reaction mixture
  2. filtrationfiltered through celite
  3. dry with materialThe filtrate was dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated
  5. distillationThe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-08c384a4b6ec466aa3f88e5e2a55a50b
Quelldatensatz
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05463118

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