Piperazine → N-1,4-Benzodioxane-2-carbonyl piperazine

HRID 428377

Reaktionsgleichung

Reaktionsgleichung von HRID 428377
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.CC[C:13]([O-:15])=O.[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1[C:13]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)=[O:15]

Komponenten

3

Edukt 2

HCID 4837PiperazineHCID 867575721,4-Benzodioxan 2-ethylcarboxylate

Produkt 1

HCID 2735449N-1,4-Benzodioxane-2-carbonyl piperazineAusbeute 94 %

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

1,4-benzodioxan-2-ethylcarboxylate, (31.2 g, 150 -mmol) and piperazine (15.5 g, 180 mmol) were stirred under nitrogen and heated to 110° C. After 5 hours, the reaction was completed, which was confirmed by thin film chromatography. The crude product was cooled to room temperature, extracted with chloroform, washed with NaHCO3 solution and water. The organic layer was dried with anhydrous sodium sulfate, filtered to afford 34.96 g of compound 1 (94% yield).

Aufarbeitung

  1. extractionextracted with chloroform
  2. washwashed with NaHCO3 solution and water
  3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-3c3d3f1904a748bd821cb7e2c09615ab
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313294B1

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