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1-Piperazinecarboxylic acid, ethyl ester → 1-Carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine

HRID 1075861
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1075861
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[CH:13][C:14]([CH3:16])=[CH:15][C:9]=3[CH2:8][C:7](=O)[C:6]=2[CH:18]=1.[C:19]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20].C(=O)(O)[O-].[Na+]>[Ti](Cl)(Cl)(Cl)Cl.C1C=CC=CC=1>[C:19]([N:24]1[CH2:29][CH2:28][N:27]([C:7]2[C:6]3[CH:18]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=3[S:11][C:10]3[CH:12]=[CH:13][C:14]([CH3:16])=[CH:15][C:9]=3[CH:8]=2)[CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]
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Komponenten

6

Edukt 3

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 516892Sodium BicarbonateHCID 214160928-chloro-2-methyl-dibenzo[b,f]thiepin-10(11H)-one

Produkt 1

HCID 214161321-Carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24193Titanium Tetrachloride
Katalysator
HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

111.4 G. of 8-chloro-2-methyl-dibenzo[b,f]thiepin-10(11H)-one in 1 l. of absolute benzene are mixed together with 268 ml. of carbethoxypiperazine and within 1 hour at 20°-25° with a solution of 65 ml. of titanium tetrachloride in 500 ml. of absolute benzene. The resulting reaction mixture thereafter is heated under reflux conditions over a period of 20 hours. The reaction mixture is then poured over a mixture of 500 ml. of saturated aqueous sodium bicarbonate solution and 700 ml. of water with strong stirring, subsequently filtered, and washed again with chloroform. After an equilibrium is reached between both phases, the organic phase is dried and evaporated, whereby there is obtained 1-carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine as a dark brown viscous oil.

Aufarbeitung

  1. customThe resulting reaction mixture
  2. temperaturethereafter is heated under reflux conditions over a period of 20 hours
  3. additionThe reaction mixture is then poured over a mixture of 500 ml
  4. filtrationof water with strong stirring, subsequently filtered
  5. washwashed again with chloroform
  6. customthe organic phase is dried
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-4815de81cacf46e9b16de0e70a818157
Quelldatensatz
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03954764

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