Sodium periodate → HCID 44218659, Verbindung

HRID 39225

Reaktionsgleichung

Reaktionsgleichung von HRID 39225
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10]([N:13]2[CH2:17][CH2:16][S:15][CH2:14]2)(=[O:12])=[O:11])[C:3]=1[C:4]#[N:5].I([O-])(=O)(=O)=[O:19].[Na+]>CO.O>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10]([N:13]2[CH2:17][CH2:16][S:15](=[O:19])[CH2:14]2)(=[O:12])=[O:11])[C:3]=1[C:4]#[N:5]

Komponenten

5

Edukt 2

HCID 23667635Sodium periodateHCID 442186552-Fluoro-6-(thiazolidine-3-sulfonyl)-benzonitrile

Produkt 1

HCID 44218659HCID 44218659, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

54 mg of 2-Fluoro-6-(thiazolidine-3-sulfonyl)-benzonitrile in 10 ml of methanol and 1 ml of water are treated with 45 mg of sodium periodate, and the mixture is stirred for 14 hours at room temperature. The reaction mixture is poured into water, and the aqueous layer is extracted three times with ethyl acetate. The combined organic layers are dried over sodium sulfate, filtered and concentrated in vacuo. Purification by reverse phase HPLC affords 40 mg of 2-Fluoro-6-(1-oxo-1 lambda*4*-thiazolidine-3-sulfonyl)-benzonitrile.

Aufarbeitung

  1. extractionthe aqueous layer is extracted three times with ethyl acetate
  2. dry with materialThe combined organic layers are dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurification by reverse phase HPLC

Quellen und Nachweise

ORD-Eintrag
ord-fd5234d09edb41feb82f3dd1a0012650
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524896B2

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