Hydrochloric Acid → Hydrazine,1,2-bis(2-chlorophenyl)-

HRID 616562

Reaktionsgleichung

Reaktionsgleichung von HRID 616562
[SH-].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+].[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N+:17](=[N:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1Cl)[O-].N1CCOCC1.[ClH:33]>>[Cl:33][N:17]([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[Cl:10])[NH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

Komponenten

6

Edukt 5

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 24477Sodium ThiosulfateHCID 28015Sodium hydrosulfideHCID 83576Diazene, 1,2-bis(2-chlorophenyl)-, 1-oxide

Produkt 1

HCID 20508459Hydrazine,1,2-bis(2-chlorophenyl)-Ausbeute 79 %

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

84 Parts of an aqueous solution of technical sodium hydrosulfide, free from sodium thiosulphate, were added to a mixture comprising 53.4 parts of 2,2'-dichloroazoxybenzene in 140 parts of morpholine at 60° C - 65° C within 90 minutes. Subsequently, the reaction temperature was raised to 75° C and maintained at that temperature for 2 1/2 hours. Next the temperature was further raised to 90° C and maintained at that temperature for 1 hour. The pH of the reaction mixture varied between 9.5 to 10. After this period the absence of the starting material was confirmed. Then the reaction mixture was cooled to 20° C and neutralized cautiously with 400 parts of hydrochloric acid of 15 percent strength at a temperature below 20° C. Then the reaction mixture was cooled to 0° C to 5° C, and the resulting precipiatate filtered off and washed with water until free of chloride. After drying below 70° C, 40.1 parts of 2,2'-dichlorohydrazobenzene of a melting point of 85° C to 87° C were obtained, this representing a yield of 79 percent of the theory.

Aufarbeitung

  1. customat 60° C - 65° C
  2. customwithin 90 minutes
  3. temperaturemaintained at that temperature for 2 1/2 hours
  4. temperatureNext the temperature was further raised to 90° C
  5. temperaturemaintained at that temperature for 1 hour
  6. waitAfter this period the absence of the starting material was confirmed
  7. temperatureThen the reaction mixture was cooled to 0° C to 5° C
  8. filtrationthe resulting precipiatate filtered off
  9. washwashed with water until free of chloride
  10. customAfter drying below 70° C

Quellen und Nachweise

ORD-Eintrag
ord-e6fe83f047ad4551a0d7896b7141b4e4
Quelldatensatz
uspto-grants-1978_02
Patentnummer
US04075198

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