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Triethylamine → 2-(2'-Nitro-4'-methylsulfonylbenzoyl)-4-propargyl-1,3-cyclohexanedione

HRID 358543
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 358543
[CH2:1]([CH:4]1[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][C:5]1=[O:11])[C:2]#[CH:3].[CH3:12][S:13]([C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[C:18]([N+:25]([O-:27])=[O:26])[CH:17]=1)(=[O:15])=[O:14].C(N(CC)CC)C.[C-]#N.[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C>[N+:25]([C:18]1[CH:17]=[C:16]([S:13]([CH3:12])(=[O:15])=[O:14])[CH:24]=[CH:23][C:19]=1[C:20]([CH:6]1[C:5](=[O:11])[CH:4]([CH2:1][C:2]#[CH:3])[CH2:9][CH2:8][C:7]1=[O:10])=[O:21])([O-:27])=[O:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 8471TriethylamineHCID 9032Potassium CyanideHCID 2855718-Crown-6HCID 114805364-(Prop-2-yn-1-yl)cyclohexane-1,3-dioneHCID 148001864-(Methanesulfonyl)-2-nitrobenzoyl chloride

Produkt 1

HCID 200662982-(2'-Nitro-4'-methylsulfonylbenzoyl)-4-propargyl-1,3-cyclohexanedione
Ausbeute 44,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

4Propargyl-1,3-cyclohexanedione (3.75 g, 25 mmol) and 4-methanesulfonyl-2-nitrobenzoyl chloride (6.06 g, 23 mmol) were dissolved in acetonitrile (100 mL) at 0° C. Triethylamine (9.6 mL, 69 mmol) was added. The mixture was then stirred for 3 hours. To the mixture was then added potassium cyanide (5.0 g) and 18-crown-6 ether (0.5 g) in one portion. The mixture was stirred for 3 days. After dilution with ether, the solution was washed with 1N HC1 and extracted with 5% K2CO3. The basic extract was acidified with concentrated HC1 and extracted with diethyl ether. The ether extract was washed with brine, dried over MgSO4, and concentrated under vacuum, yielding 3.9 g of the desired product, an orange solid, m.p. 65-70° C. The structure was confirmed by nuclear magnetic spectroscopy, infrared spectroscopy, and mass spectroscopy.

Aufarbeitung

  1. stirringThe mixture was stirred for 3 days
  2. washAfter dilution with ether, the solution was washed with 1N HC1
  3. extractionextracted with 5% K2CO3
  4. extractionThe basic extract
  5. extractionextracted with diethyl ether
  6. extractionThe ether extract
  7. washwas washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-920785c218cf4fe790f3acaf11cbf2de
Quelldatensatz
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04997473

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