1-Methylpiperazine → HCID 22767842, Verbindung

HRID 372450Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 372450
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:14]=[CH:15][C:16]([CH3:18])=[CH:17][C:4]=2[CH2:3]1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(Cl)(Cl)Cl>[CH3:18][C:16]1[CH:15]=[CH:14][C:5]2[O:6][C:7]3[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][C:8]=3[CH:2]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH2:3][C:4]=2[CH:17]=1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 2276790610-Chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin

Produkt 1

HCID 22767842HCID 22767842, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

0.8 G. of 10-chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin and 0.58 g. of 1-methyl-piperazine are dissolved in 4 ml. of chloroform and heated at reflux for 21 hours. Then, the chloroform is evaporated in vacuo. The residue is partitioned between benzene and aqueous sodium carbonate solution. The benzene solution is extracted with dilute hydrochloric acid. The hydrochloric acid extract is made alkaline with sodium carbonate and extracted with benzene. Thereafter, the benzene extract is washed several times with water, dried over sodium sulfate, evaporated in vacuo, and there is obtained 1-[10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin-10-yl]-4-methyl-piperazine, the dihydrochloride of which melts at 197°-198° C. (with decomposition).

Aufarbeitung

  1. temperatureat reflux for 21 hours
  2. customThen, the chloroform is evaporated in vacuo
  3. customThe residue is partitioned between benzene and aqueous sodium carbonate solution
  4. extractionThe benzene solution is extracted with dilute hydrochloric acid
  5. extractionThe hydrochloric acid extract
  6. extractionextracted with benzene
  7. extractionThereafter, the benzene extract
  8. washis washed several times with water
  9. dry with materialdried over sodium sulfate
  10. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b8e746b684ae4d61aed3c2463f1e1928
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04091023

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