Water → HCID 178460141, Verbindung

HRID 1493506Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1493506
[C:1]([CH:5]1[C:10](=[O:11])[CH2:9][CH:8]([CH2:12][CH2:13][S:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][CH:16]=2)[CH2:7][C:6]1=[O:25])(=O)[CH2:2][CH3:3].Cl.[CH2:27]([O:30][NH2:31])[CH:28]=[CH2:29].C(N(CC)CC)C.O>C(O)C>[CH2:27]([O:30][NH:31][C:1](=[C:5]1[C:6](=[O:25])[CH2:7][CH:8]([CH2:12][CH2:13][S:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][CH:16]=2)[CH2:9][C:10]1=[O:11])[CH2:2][CH3:3])[CH:28]=[CH2:29]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 3084724O-Allylhydroxylamine hydrochlorideHCID 15017462HCID 15017462, Verbindung

Produkt 1

HCID 178460141HCID 178460141, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

0.19 Gram of 2-propionyl-5-[2-(4-trifluoromethylphenylthio)ethyl]cyclohexane-1,3-dione was dissolved in 5 ml of ethanol, and 0.07 g of allyloxyamine hydrochloride and 0.06 g of triethylamine were added to the resulting solution which was then stirred overnight at room temperature. The reaction solution was poured into water, acidified and extracted with chloroform. After removing chloroform, the residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1) to obtain 0.13 g of 2-(1-allyloxyaminopropylidene)5-[2-(4-trifluoromethylphenylthio)ethyl]cyclohexane-1,3-dione.

Aufarbeitung

  1. extractionextracted with chloroform
  2. customAfter removing chloroform
  3. customthe residue was purified by thin layer chromatography (eluent, hexane:ethyl acetate=5:1)

Quellen und Nachweise

ORD-Eintrag
ord-af35644d9bea450da5ce4f4b3f90b2c7
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05021579

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