Water → HCID 58994992, Verbindung

HRID 1054278Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1054278
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2([C:18]#[N:19])[CH2:15][CH2:14][S:13](=[O:17])(=[O:16])[CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH2:20]>C(O)C.CCOC(C)=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2([C:18]([NH2:19])=[O:20])[CH2:11][CH2:12][S:13](=[O:17])(=[O:16])[CH2:14][CH2:15]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

Komponenten

5

Edukt 2

HCID 962WaterHCID 589949324-(4-Nitro-phenyl)-1,1-dioxo-hexahydro-1lambda6-thiopyran-4-carbonitrile

Produkt 1

HCID 58994992HCID 58994992, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of 4-(4-nitro-phenyl)-1,1-dioxo-hexahydro-1λ6-thiopyran-4-carbonitrile (as prepared in the previous step) in ethanol and water is treated with NaBO3 (Synthetic Communications, 20(4), 563-71, (1990)). The mixture is diluted with EtOAc and washed with water. The organic layer is dried (MgSO4) and concentrated in vacuo. The residue is purified by silica gel chromatography with the appropriate solvent to afford the title compound.

Aufarbeitung

  1. washwashed with water
  2. dry with materialThe organic layer is dried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe residue is purified by silica gel chromatography with the appropriate solvent

Quellen und Nachweise

ORD-Eintrag
ord-e7058be0381444c3b983310c1caf07f3
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394289B2

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