Stannous Chloride → HCID 178482256, Verbindung

HRID 1189673Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1189673
[F:1][C:2]([F:29])([F:28])[C@H:3]1[CH2:8][CH2:7][C@H:6]([NH:9][C:10](=[O:27])[C:11]2[CH:16]=[C:15]([N+:17]([O-])=O)[C:14]([NH:20][CH3:21])=[CH:13][C:12]=2[N:22]([CH3:26])[CH2:23][C:24]#[N:25])[CH2:5][CH2:4]1.Cl[Sn]Cl>CCOC(C)=O>[F:1][C:2]([F:28])([F:29])[C@H:3]1[CH2:8][CH2:7][C@H:6]([NH:9][C:10](=[O:27])[C:11]2[CH:16]=[C:15]([NH2:17])[C:14]([NH:20][CH3:21])=[CH:13][C:12]=2[N:22]([CH3:26])[CH2:23][C:24]#[N:25])[CH2:5][CH2:4]1

Komponenten

4

Edukt 2

HCID 24479Stannous ChlorideHCID 178482257HCID 178482257, Verbindung

Produkt 1

HCID 178482256HCID 178482256, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A mixture of N-(trans-4-trifluoromethyl-cyclohexyl)-2-[N-methyl-N-cyanomethyl-amino]-4-methylamino-5-nitro-benzoic acid amide (50 mg, 0.12 mmol), SnCl2 (134 mg 0.59 mmol and 5 mL EtOAc is stirred at reflux for 4 h. The mixture is diluted with EtOAc, washed with sat aq NaHCO3, filtered through a pad of celite and the celite pad is washed with EtOAc. The combined organic phases are dried with Na2SO4, filtered and concentrated.

Aufarbeitung

  1. temperatureat reflux for 4 h
  2. washwashed with sat aq NaHCO3
  3. filtrationfiltered through a pad of celite
  4. washthe celite pad is washed with EtOAc
  5. dry with materialThe combined organic phases are dried with Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-f1d71812215d46a7b0880284f09eb468
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08674113B2

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