Ethylenediamine → 4-(2-Imidazolin-2-YL)-7-methylchromane
Reaktionsgleichung
CO[C:3]1[CH:12]=[C:11]2[C:6](C[CH2:8][CH2:9][CH:10]2[C:13]#[N:14])=[CH:5][C:4]=1[CH3:15].[CH2:16]([NH2:19])[CH2:17]N.C1(C)C=CC(S(O)(=O)=[O:27])=CC=1>>[NH:19]1[CH2:16][CH2:17][N:14]=[C:13]1[CH:10]1[C:11]2[C:6](=[CH:5][C:4]([CH3:15])=[CH:3][CH:12]=2)[O:27][CH2:8][CH2:9]1Komponenten
4
Versuchsvorschrift
This compound was prepared in a manner analogous to that of Step G of Example 1, by the reaction of 0.6 gram (0.003 mole) of 7-methylchromane-4-carbonitrile (iv) and 2 grams (0.008 mole) of the ethylenediamine salt of p-toluenesulfonic acid (prepared in Step F of Example 1). The reaction product was purified by column chromatography on Grade II basic alumina (3% water) using mixtures of methylene chloride and methanol as an eluant. The appropriate fractions of eluate were combined and concentrated under reduced pressure, yielding 0.25 gram of subject compound. The NMR spectrum was consistent with the proposed structure.
Aufarbeitung
- customThis compound was prepared in a manner analogous to that of Step G of Example 1
- customThe reaction product was purified by column chromatography on Grade II basic alumina (3% water)
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-766b774349ba40bea1b4ff814c478428
- Quelldatensatz
- uspto-grants-2008_08
- Patentnummer
- US07417057B2
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