1-(3-Chlorophenyl)piperazine monohydrochloride → 8-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate

HRID 1761436Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1761436
Br[CH2:2][CH2:3][CH2:4][O:5][N:6]1[C:15](=[O:16])[CH2:14][C:9]2([CH2:13][CH2:12][CH2:11][CH2:10]2)[CH2:8][C:7]1=[O:17].[ClH:18].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1>CCN(CC)CC>[OH2:5].[ClH:19].[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[Cl:19][C:20]1[CH:21]=[C:22]([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][N:6]3[C:15](=[O:16])[CH2:14][C:9]4([CH2:13][CH2:12][CH2:11][CH2:10]4)[CH2:8][C:7]3=[O:17])[CH2:28][CH2:27]2)[CH:23]=[CH:24][CH:25]=1.[ClH:18]

Komponenten

4

Edukt 2

HCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 142805838-(3-Bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione

Produkt 1

HCID 1317157328-[3-[4-(3-Chlorophenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A solution of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (4.0 g) and 1-(3-chlorophenyl)piperazine hydrochloride (3.06 g) in 50 ml of Et3N was heated to reflux with stirring under N2. After 1 hour TLC (thin layer chromatography) showed the absence of starting material. The excess Et3N was removed in vacuo and the residue chromatographed on silica using ethyl acetate as the eluent. Fractions containing the desired product were combined and concentrated in vacuo.

Aufarbeitung

  1. temperatureto reflux
  2. customThe excess Et3N was removed in vacuo
  3. customthe residue chromatographed on silica
  4. additionFractions containing the desired product
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c55a9c5047b041e78a0ff6d57ab68f58
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04826846

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