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Piperazine → 4-Methyl-10-(1-piperazinyl)-4H-thieno[3,4-b][1,5]benzodiazepine fumarate

HRID 371648
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 371648
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5](SC)[C:4]2=[CH:15][S:16][CH:17]=[C:3]12.[NH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C1(C)C(C)=CC=CC=1.[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]/[C:35]([OH:37])=[O:36]>C(O)(=O)C.C(O)C>[C:32]([OH:39])(=[O:38])/[CH:33]=[CH:34]/[C:35]([OH:37])=[O:36].[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[C:4]2=[CH:15][S:16][CH:17]=[C:3]12
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 4837PiperazineHCID 7237O-XyleneHCID 444972Fumaric AcidHCID 125216604-Methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

Produkt 1

HCID 125216894-Methyl-10-(1-piperazinyl)-4H-thieno[3,4-b][1,5]benzodiazepine fumarate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176
Acetic Acid
Katalysator
HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A mixture comprising 2.6 g. of 4-methyl-10-(methylthio)-4H-thieno[3,4-b][1,5]benzodiazepine (U.S. Pat. No. 3,951,981 -- Ex. 7), 8.6 g. of piperazine, 3 drops of acetic acid and 15 ml. of xylene is stirred and refluxed for 4 hours. The reaction mixture is evaporated, washed with water and the residue is dissolved in 50 ml. of 2N acetic acid. The solution is filtered, the filtrate is made alkaline with ammonium hydroxide and extracted with benzene. The extracts are dried over magnesium sulfate, filtered and evaporated producing an amber oil. This oil is dissolved in 20 ml. of ethanol and a mixture of 2.1 g. of fumaric acid in 40 ml. of ethanol is added. The solid is collected and recrystallized from 125 ml. of methanol giving the desired product as the fumarate salt, m.p. 205°-206° C. (dec.).

Aufarbeitung

  1. temperaturerefluxed for 4 hours
  2. customThe reaction mixture is evaporated
  3. washwashed with water
  4. dissolutionthe residue is dissolved in 50 ml
  5. filtrationThe solution is filtered
  6. extractionextracted with benzene
  7. dry with materialThe extracts are dried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated
  10. customproducing an amber oil
  11. dissolutionThis oil is dissolved in 20 ml
  12. customThe solid is collected
  13. customrecrystallized from 125 ml

Quellen und Nachweise

ORD-Eintrag
ord-e1d5247890034975b3d50245f834917e
Quelldatensatz
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04087421

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