Hydrochloric Acid → Phenyl 3-methyl-3-nitrobutane-1-sulfonate

HRID 501243

Reaktionsgleichung

Reaktionsgleichung von HRID 501243
[CH:1]([S:3]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:5])=[O:4])=[CH2:2].[N+:13]([CH:16]([CH3:18])[CH3:17])([O-:15])=[O:14].C(N(C(C)C)C(C)C)C.Cl>CC(=O)OCC>[CH3:17][C:16]([N+:13]([O-:15])=[O:14])([CH3:18])[CH2:2][CH2:1][S:3]([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:4])=[O:5]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3982-NitropropaneHCID 81531DiisopropylethylamineHCID 564920Phenyl ethenesulfonate

Produkt 1

HCID 86616499Phenyl 3-methyl-3-nitrobutane-1-sulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 9.43 g of phenyl ethenesulfonate and 4.60 ml of 2-nitro-propane was heated to 80° C. and, at 80° C., 0.89 ml of ethyidiisopropylamine was added dropwise. The mixture was stirred at 80° C. for 4 hours and 30 minutes, left to stand at RT for 16 hours and then stirred at 80° C. for a further 2 hours. Cooling to RT was followed by addition of 250 ml of a 2N aqueous HCl solution and extraction 3 times with 150 ml of EA each time. Drying over Na2SO4 and removal of the solvent in vacuo were followed by coevaporation 3 times with 100 ml of toluene each time. 13.47 g of a pale yellow oil were obtained.

Aufarbeitung

  1. waitleft
  2. waitto stand at RT for 16 hours
  3. stirringstirred at 80° C. for a further 2 hours
  4. temperatureCooling to RT
  5. dry with materialDrying over Na2SO4 and removal of the solvent in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-6087daf0a21747a5a9e520a04e85a4ec
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772262B2

Verknüpfte Notizen

Wird geladen…