Formaldehyde → 5H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)-

HRID 1768655Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1768655
[CH:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.[CH2:23]=O>ClC(Cl)C.C(O)(=O)C>[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][C:2]2[CH:3]=[CH:4][C:5]3[NH:6][C:7]4[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=4[CH2:9][CH2:10][C:11]=3[CH:1]=2)[CH2:19][CH2:18]1

Komponenten

6

Edukt 3

HCID 712FormaldehydeHCID 10308IminodibenylHCID 531671-Methylpiperazine

Produkt 1

HCID 30488975H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)-Ausbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 63651,1-DichloroethaneLösungsmittel

Versuchsvorschrift

10,11-Dihydro-5H-dibenz [b,f]azepine (250 g) was suspended in a mixture of 600 ml of dichloroethane and 600 ml of acetic acid, and 155 ml of 1-methylpiperazine was added dropwise to the suspension. To the mixture was added 42 g of paraformaldehyde at 50° C. followed by stirring for 6 hours. The solvent was distilled off under reduced pressure and the residue was diluted with ethyl acetate. The solution was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the product (91%). The obtained product was subjected to the subsequent reaction without particular purification.

Aufarbeitung

  1. additionwas added dropwise to the suspension
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washThe solution was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cf011155c84141b59138b5163e9ca8dd
Quelldatensatz
uspto-grants-1995_01
Patentnummer
US05378701

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