Sodium Iodide → HCID 20636318, Verbindung

HRID 49329

Reaktionsgleichung

Reaktionsgleichung von HRID 49329
CS([O:5][CH2:6][C:7]1[S:8][C:9]([C:12]2([CH2:17][CH3:18])[O:16][CH2:15][CH2:14][O:13]2)=[CH:10][CH:11]=1)(=O)=O.O[C:20]1[CH:21]=[C:22]([C:30]([O:32][CH3:33])=[O:31])[C:23](=[CH:28][CH:29]=1)[C:24]([O:26][CH3:27])=[O:25].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CC(=O)CC>[CH2:17]([C:12]1([C:9]2[S:8][C:7]([CH2:6][O:5][C:29]3[CH:28]=[C:23]([C:24]([O:26][CH3:27])=[O:25])[C:22](=[CH:21][CH:20]=3)[C:30]([O:32][CH3:33])=[O:31])=[CH:11][CH:10]=2)[O:16][CH2:15][CH2:14][O:13]1)[CH3:18]

Komponenten

6

Edukt 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 89726Dimethyl 4-hydroxyphthalateHCID 206363015-(2-Ethyl-[1,3]dioxolan-2-yl)-2-thienylmethyl methanesulphonate

Produkt 1

HCID 20636318HCID 20636318, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

9.25 g (43.2 mmol) of 5-(2-ethyl-[1,3]dioxolan-2-yl)-2-thienylmethyl methanesulphonate are dissolved in 100 mL of 2-butanone, and 9.07 g (43.2 mmol) of dimethyl 4-hydroxyphthalate (prepared in Example 1(b)), 6 g of potassium carbonate (43.2 mmol) and 20 mg of sodium iodide are added. The mixture is refluxed for 12 hours, cooled and filtered. The filtrate is concentrated under reduced pressure and then purified by chromatography on a column of silica. A yellow oil is obtained (m=12.70 g; Y=73%).

Aufarbeitung

  1. temperatureThe mixture is refluxed for 12 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. custompurified by chromatography on a column of silica
  6. customA yellow oil is obtained (m=12.70 g; Y=73%)

Quellen und Nachweise

ORD-Eintrag
ord-3398eeb0de564ba9ab1b8cc49873e73a
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06706725B1

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