N-(5-Chloro-2-methylphenyl)piperazine → 8-{2-[4-(5-Chloro-2-methylphenyl)piperazino]ethyl}-8-azaspiro[4.5]decane-7,9-dione
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:14])=[C:6]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:7]=1.Cl[CH2:16][CH2:17][N:18]1[C:27](=[O:28])[CH2:26][C:21]2([CH2:25][CH2:24][CH2:23][CH2:22]2)[CH2:20][C:19]1=[O:29]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:14])=[C:6]([N:8]2[CH2:9][CH2:10][N:11]([CH2:16][CH2:17][N:18]3[C:19](=[O:29])[CH2:20][C:21]4([CH2:25][CH2:24][CH2:23][CH2:22]4)[CH2:26][C:27]3=[O:28])[CH2:12][CH2:13]2)[CH:7]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 160 °C
Versuchsvorschrift
A mixture of 1-(5-chloro-2-methylphenyl)piperazine (20 mg, 0.095 mmol) and 8-(2-chloroethyl)-8-azaspiro[4.5]decane-7,9-dione(20 mg, 0.087 mmol) was heated with stirring at 160° C. for 5 hours. The residue was purified by preparative HPLC (see Example 8 for conditions), giving (after removal of the solvent) the title compound as a pale yellow oil (17.3 mg, 0.043 mmol, 49%): ESI-MS m/z 404 (MH+).
Aufarbeitung
- temperaturewas heated
- customThe residue was purified by preparative HPLC (see Example 8 for conditions)
- customgiving (
Quellen und Nachweise
- ORD-Eintrag
- ord-8ed87a0303924bdb9d401702469b228a
- Quelldatensatz
- uspto-grants-2004_03
- Patentnummer
- US06706716B2
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