Triacetoxyperiodinane → HCID 71205441, Verbindung

HRID 2280858Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2280858
[OH:1][CH:2]1[CH2:5][N:4]([C:6]2[CH:7]=[C:8]([CH:13]=[CH:14][CH:15]=2)[C:9]([O:11][CH3:12])=[O:10])[CH2:3]1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[O:1]=[C:2]1[CH2:5][N:4]([C:6]2[CH:7]=[C:8]([CH:13]=[CH:14][CH:15]=2)[C:9]([O:11][CH3:12])=[O:10])[CH2:3]1

Komponenten

4

Edukt 2

HCID 159087TriacetoxyperiodinaneHCID 71205443HCID 71205443, Verbindung

Produkt 1

HCID 71205441HCID 71205441, VerbindungAusbeute 75,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of compound 3a (1.60 g, 7.7 mmol) in dry DCM (30 mL) was added Dess-Martin periodinane (6.5 g, 15.4 mmol) at 0° C. and the mixture was stirred at rt for 2 h under N2 atmosphere. The mixture was quenched with saturated sodium bicarbonate solution and diluted with EA. The organic portion was washed with brine, dried over Na2SO4, filtered, concentrated under reduced pressure and purified by CC (PE/EA=4:1) to give compound 3 (1.2 g, 75%) as a white solid.

Aufarbeitung

  1. customThe mixture was quenched with saturated sodium bicarbonate solution
  2. additiondiluted with EA
  3. washThe organic portion was washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. custompurified by CC (PE/EA=4:1)

Quellen und Nachweise

ORD-Eintrag
ord-33fc94a1f17744a08d4a28132405c93e
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09139539B2

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