Potassium Iodide → L82Nub8C3A

HRID 18845

Reaktionsgleichung

Reaktionsgleichung von HRID 18845
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:5][CH:4]=1.[C:17](=[O:20])([O-:19])[O-].[K+].[K+].[I-].[K+].[CH3:25][O:26][C:27](=[O:33])[C@H:28]([CH:30]([CH3:32])[CH3:31])[NH2:29]>C(#N)C>[C:27]([OH:33])(=[O:26])[C:17]([OH:19])=[O:20].[CH3:25][O:26][C:27](=[O:33])[C@H:28]([CH:30]([CH3:32])[CH3:31])[NH:29][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:15]#[N:16])=[CH:5][CH:4]=1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 94285Valine methyl esterHCID 15019124'-(Bromomethyl)-2-cyanobiphenyl

Produkt 1

HCID 51050401L82Nub8C3A

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
42.5 °C

Versuchsvorschrift

100 g 4-Bromomethyl-2′-cyanobiphenyl is added to 500 ml acetonitrile followed by 69 g of anhydrous potassium carbonate, 12 g potassium iodide and 65 g L-Valine methyl ester. The reaction mixture is stirred at 40-45° C. for 3-4 hours. After completion of the reaction, the reaction mixture is filtered and acetonitrile is removed under vacuum at 45-50° C. 300 ml of water and 300 ml of o-xylene are added to the residue and the layers are separated. Solution of 50 g oxalic acid in 500 ml water is added to the organic layer and stirred for about an hour and filtered. The solid is washed and then dried under vacuum at 50-55° C. (yield: 130-135 g).

Aufarbeitung

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture is filtered
  3. customacetonitrile is removed under vacuum at 45-50° C
  4. addition300 ml of water and 300 ml of o-xylene are added to the residue
  5. customthe layers are separated
  6. additionSolution of 50 g oxalic acid in 500 ml water is added to the organic layer
  7. stirringstirred for about an hour
  8. filtrationfiltered
  9. washThe solid is washed
  10. customdried under vacuum at 50-55° C. (yield: 130-135 g)

Quellen und Nachweise

ORD-Eintrag
ord-c3a69816ee7642f9abb9b3e867e8099c
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741507B2

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