Water → HCID 178460141, Verbindung

HRID 703283

Reaktionsgleichung

Reaktionsgleichung von HRID 703283
[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-bc7a3f2e6566429fbcd1c03bf193c0ea
Quelldatensatz
uspto-grants-1991_01
Patentnummer
US04981971

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