Sodium hydride → HCID 178514754, Verbindung

HRID 574904Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 574904
[Si]([O:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][OH:16])[CH2:11][CH2:10]1)(C(C)(C)C)(C)C.[Cl:17][C:18]1[CH:19]=[C:20]([S:25]([NH2:28])(=[O:27])=[O:26])[CH:21]=[CH:22][C:23]=1F.[H-].[Na+]>O1CCCC1>[Cl:17][C:18]1[CH:19]=[C:20]([S:25]([NH2:28])(=[O:26])=[O:27])[CH:21]=[CH:22][C:23]=1[O:16][CH2:15][C@H:12]1[CH2:11][CH2:10][C@H:9]([OH:8])[CH2:14][CH2:13]1

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 75098833-Chloro-4-fluorobenzenesulfonamideHCID 178455322HCID 178455322, Verbindung

Produkt 1

HCID 178514754HCID 178514754, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

(Trans-4-(tert-butyldimethylsilyloxy)cyclohexyl)methanol (275 mg, prepared according to a procedures in WO 2008/124878) and 3-chloro-4-fluorobenzenesulfonamide (259 mg) in tetrahydrofuran (15 mL) were treated with sodium hydride (180 mg, 60%) overnight. The reaction was quenched with water (1 mL) and trifluoroacetic acid (4 mL) was added. The resulting mixture was stirred for 1 hour and concentrated. The residue was triturated with water and methanol to provide the title compound.

Aufarbeitung

  1. customThe reaction was quenched with water (1 mL) and trifluoroacetic acid (4 mL)
  2. additionwas added
  3. concentrationconcentrated
  4. customThe residue was triturated with water and methanol

Quellen und Nachweise

ORD-Eintrag
ord-00e4ab8248444244a97713ab634c5cd5
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09034875B2

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