Sodium Hydroxide → HCID 21555785, Verbindung

HRID 2296067Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2296067
C(OC([C:6]1[N:10]2[C:11]3[CH:25]=[CH:24][C:23](Cl)=[CH:22][C:12]=3[C:13](C3C=CC=CC=3)=[N:14][CH2:15][C:9]2=NN=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-:33].[Na+]>O1CCCC1>[N:10]1([CH2:6][OH:33])[C:11]2[CH:25]=[CH:24][CH:23]=[CH:22][C:12]=2[CH:13]=[N:14][CH:15]=[CH:9]1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 13060131Ethyl 8-chloro-6-phenyl-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepine-1-carboxylateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 21555785HCID 21555785, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 0.37 g of 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxylic acid ethyl ester in 5 ml of absolute tetrahydrofuran is added dropwise in the course of 15 minutes, with ice cooling and with stirring, to a suspension of 0.078 g of lithium aluminium hydride in 5 ml of absolute tetrahydrofuran. After a further 45 minutes of stirring at 0°-5°, 0.40 ml of 1-n sodium hydroxide solution are added dropwise. The inorganic salts are filtered off, the filtrate is concentrated in vacuo, and the residue dissolved in 10 ml of chloroform. The solution is washed with 1-n sodium hydroxide solution and then with water, dried over sodium sulphate, and concentrated by evaporation. The residue is recrystallised from ethyl acetate/petroleum ether to obtain 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4benzodiazepine-1-methanol, M.P. 210°-211°.

Aufarbeitung

  1. filtrationThe inorganic salts are filtered off
  2. concentrationthe filtrate is concentrated in vacuo
  3. dissolutionthe residue dissolved in 10 ml of chloroform
  4. washThe solution is washed with 1-n sodium hydroxide solution
  5. dry with materialwith water, dried over sodium sulphate
  6. concentrationconcentrated by evaporation
  7. customThe residue is recrystallised from ethyl acetate/petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-84d1484bad754c9db4f4186212687d11
Quelldatensatz
uspto-grants-1984_01
Patentnummer
US04427590

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