Sodium Hydroxide → (4-Benzylpiperazin-1-yl)(cyclohexyl)methanone

HRID 2412392

Reaktionsgleichung

Reaktionsgleichung von HRID 2412392
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:14]1([C:20](Cl)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.[OH-].[Na+]>C(Cl)(Cl)Cl.O>[CH:14]1([C:20]([N:11]2[CH2:12][CH2:13][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9][CH2:10]2)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 75938Cyclohexanecarbonyl chlorideHCID 759941-Benzylpiperazine

Produkt 1

HCID 562738(4-Benzylpiperazin-1-yl)(cyclohexyl)methanoneAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

To a solution of 21.2 g (0.12 mole) of 1-benzylpiperazine in 100 ml of CHCl3 was added dropwise over a period of 30 minutes a solution of 15.0 g (0.10 mole) of cyclohexanecarbonyl chloride in 50 ml of CHCl3. The mixture was allowed to stand at room temperature during 45 minutes and was made basic with 5 g of sodium hydroxide in 50 ml of water. The nonaqueous layer was separated, dried over sodium sulphate and concentrated. The residue was distilled b.p. 150°-56° C. at 0.1-0.2 mmHg to give 21.2 g of 1-cyclohexanecarbonyl-4-benzylpiperazine.

Aufarbeitung

  1. customThe nonaqueous layer was separated
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated
  4. distillationThe residue was distilled b.p. 150°-56° C. at 0.1-0.2 mmHg

Quellen und Nachweise

ORD-Eintrag
ord-2f49ef55eced435db77d406044c58ef4
Quelldatensatz
uspto-grants-1985_01
Patentnummer
US04492698

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