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Sodium Sulfite → HCID 90449435, Verbindung

HRID 1411297
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1411297
[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH:17]([OH:19])[CH3:18])[CH:15]=3)[N:10]([C:20]([NH:22][C:23]3[S:24][C:25]([Cl:28])=[CH:26][N:27]=3)=[O:21])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.S([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:17](=[O:19])[CH3:18])[CH:15]=3)[N:10]([C:20]([NH:22][C:23]3[S:24][C:25]([Cl:28])=[CH:26][N:27]=3)=[O:21])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24437Sodium SulfiteHCID 159087TriacetoxyperiodinaneHCID 90449833HCID 90449833, Verbindung

Produkt 1

HCID 90449435HCID 90449435, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The 1′-acetyl-N-(5-chlorothiazol-2-yl)-5-(1-hydroxyethyl)spiro[indoline-3,3′-pyrrolidine]-1-carboxamide (22.3 mg, 0.053 mmol) obtained in Step 2 of Example 401 was dissolved in methylene chloride (0.5 mL). Thereafter, Dess-martin periodinane (27.0 mg, 0.0635 mmol) was added to the above obtained solution at room temperature, and the thus obtained mixture was then stirred at the same temperature as above for 1 hour. Thereafter, an aqueous solution of sodium sulfite was added to the reaction solution, and the mixed solution was then extracted with chloroform. The organic layer was washed with brine, and was then dried over anhydrous sodium sulfate, followed by concentration in vacuo. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=10:1) to obtain the captioned compound (21.7 mg, 99%) in the form of a white solid.

Aufarbeitung

  1. extractionthe mixed solution was then extracted with chloroform
  2. washThe organic layer was washed with brine
  3. dry with materialwas then dried over anhydrous sodium sulfate
  4. concentrationfollowed by concentration in vacuo
  5. customThe obtained residue was purified by silica gel column chromatography (chloroform:methanol=10:1)

Quellen und Nachweise

ORD-Eintrag
ord-ae131e6b4a6d43efb6671d4a67e0fc96
Quelldatensatz
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08921576B2

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