Reaktionsgleichung
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O.S(Cl)(Cl)=O.Cl.[CH3:20][NH:21][OH:22].C(=O)([O-])[O-].[K+].[K+]>>[CH3:20][N:21]([C:12](=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][Br:1])[OH:22]Komponenten
Versuchsvorschrift
According to the procedure shown in Example 11, 2.65 g (10 mmol) of 11-bromoundecanoic acid (IV5) was treated with 1 ml of thionyl chloride and the resulting product was treated with 850 mg (10.2 mmol) of methylhydroxylamine hydrochloride and 1.5 g (10.9 mmol) of potassium carbonate to give N-methyl-11-bromoundecanohydroxamic acid (V6), which was recrystallized from a mixture of ether-n-hexane to give 2.46 g of the compound (V6) as colorless prismatic crystals in 83.6% yield. mp. 49° C. to 51° C. To a solution of 2.11 g (7.2 mmol) of the compound (V6) was allowed to react with 1.71 g (7.2 mmol) of 3,5-di-tert-butyl-4-hydroxythiophenol under the condition shown in Example 11. The prepared product was chromatographed and eluted with a mixture of ether-ethyl acetate (2:1) to give 3.12 g of the aimed compound (I13) as a pale yellow in 96.3% yield.
Quellen und Nachweise
- ORD-Eintrag
- ord-f54623565cef4901a18367f82765a24a
- Quelldatensatz
- uspto-grants-1992_02
- Patentnummer
- US05091569
Verknüpfte Notizen
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