Water → HCID 11629980, Verbindung
Reaktionsgleichung
[I-].[CH3:2][S+](C)C.[OH-].[K+].[F:8][C:9]([F:22])([F:21])[C:10]1([C:13]2[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=2)[N:12]=[N:11]1.O>C(#N)C>[O:18]1[CH2:2][CH:17]1[C:16]1[CH:19]=[CH:20][C:13]([C:10]2([C:9]([F:8])([F:21])[F:22])[N:11]=[N:12]2)=[CH:14][CH:15]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
0.95 g of trimethylsulfonium iodide and 0.52 g of potassium hydroxide were dissolved in 4 ml of acetonitrile, and agitated for 10 minutes at 60° C. in a nitrogen gas atmosphere. 1.00 g of 4-(3-trifluoromethyl-3H-diazirine-3-yl)benzaldehyde were added together with 5.3 ml of acetonitrile, then 0.02 g of water were added. This was agitated for one hour at 60° C. in a nitrogen gas atmosphere. After extracting with ethyl ether, the resulting substance was washed twice with water and once with saturated saline solution, then dried with anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure, and the resulting substance was purified by silica gel chromatography (hexane:chloroform=1:2, V/V) to obtain 0.56 g of 3-(4-oxiranylphenyl)-3-trifluoromethyl-3H-diazirine (52% yield).
Aufarbeitung
- stirringThis was agitated for one hour at 60° C. in a nitrogen gas atmosphere
- extractionAfter extracting with ethyl ether
- washthe resulting substance was washed twice with water and once with saturated saline solution
- dry with materialdried with anhydrous magnesium sulfate
- filtrationfiltered
- customThe solvent was removed under reduced pressure
- customthe resulting substance was purified by silica gel chromatography (hexane:chloroform=1:2, V/V)
Quellen und Nachweise
- ORD-Eintrag
- ord-982c4896b47741f69dd212f3f7adf5cd
- Quelldatensatz
- uspto-grants-2011_10
- Patentnummer
- US08043666B2
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