Hydrochloric Acid → HCID 58303835, Verbindung

HRID 1886981Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1886981
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:10]=1Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.O.O.O.O.O.O.O.[S-2:28].[Na+].[Na+].CCOCC.Cl>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:10]=1[SH:28])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 73972Sodium sulfide nonahydrateHCID 143561211-(Benzyloxy)-2-chloro-3-nitrobenzene

Produkt 1

HCID 58303835HCID 58303835, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
22 °C

Versuchsvorschrift

To a solution of 8.56 g (32.5 mmol) of 1-(benzyloxy)-2-chloro-3-nitrobenzene in 120 mL of DMF was added 15.6 g (64.9 mmol) of pulverized sodium sulfide nonahydrate. The mixture was stirred vigorously at 22° C. for 30 hours and then poured into a vigorously stirred mixture of ether and 1 N HCl. The organic layer was washed with water then brine, dried (Na2SO4), and evaporated. The residue was crystallized from dichloromethane (DCM) and hexane to give 2-(benzyloxy)-6-nitrobenzenethiol.

Aufarbeitung

  1. washThe organic layer was washed with water
  2. dry with materialbrine, dried (Na2SO4)
  3. customevaporated
  4. customThe residue was crystallized from dichloromethane (DCM) and hexane

Quellen und Nachweise

ORD-Eintrag
ord-1a9ba1d883fc4afa9f25825215dda737
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501727B2

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