Benzene → Cyclohexanone Oxime

HRID 234111

Reaktionsgleichung

[CH:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:7]1(=[N:13][OH:14])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.C1(S([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]CCCCCC)(=O)=[O:22])C=CC=CC=1.[Na]>S(=O)(=O)(O)O>[C:7]1(=[N:13][OH:14])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.[C:1]1(=[O:22])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:25]1(=[O:24])[NH:13][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

Take 200 ml of aqueous solution of 2.16N sulfuric acid in a round bottom flask. Dissolve in this solution 6.8 gm of sodium dodecyl benzene sulfonate (SDBS) and 1.3 gm of benzene by mild stirring. Keep the flask in a water bath maintained at temperature of 40° C. A macroemulsions of benzene in sulfuric acid is formed. To this macroemulsion, add 14.0 gm of cyclohexanone oxime and stir for 21/2 hours. Neutralize the excess acid using Whatman No. 1 filter paper to remove or recycle the the unreacted cyclohexanone oxime. Separate the organic and aqueous layers of the filtrate. Wash the aqueous layer with 3×10 ml benzene and add the benzene washing with the main organic layer. Analyze the benzene layer, the aqueous layer and the unreacted cyclohexanone oxime as obtained above by Gas Chromatography for the amount of cyclohexanone oxime, cyclohexanone and caprolactam.

Aufarbeitung

filtration1 filter paper
customto remove
customSeparate the organic and aqueous layers of the filtrate
washWash the aqueous layer with 3×10 ml benzene
additionadd the benzene washing with the main organic layer

Quellen und Nachweise

ORD-Eintrag: ord-27284f3f9dc54790b074b4ef57dc8990
Quelldatensatz: uspto-grants-1997_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05594137

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