Hydrochloric Acid → HCID 86616004, Verbindung

HRID 1987578Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1987578
N[C:2]1[CH:3]=[C:4]([S:9]([OH:12])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.N([O-])=O.[Na+].[CH3:18][S:19]SC>O>[Cl:8][C:7]1[CH:6]=[CH:5][C:4]([S:9]([OH:12])(=[O:11])=[O:10])=[CH:3][C:2]=1[S:19][CH3:18]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 12232Dimethyl DisulfideHCID 668174-Chlorometanilic acidHCID 23668193Sodium Nitrite

Produkt 1

HCID 86616004HCID 86616004, VerbindungAusbeute 291,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

To a solution of 3-amino-4-chloro-benzenesulfonic acid (5.00 g, 24 mmol) in distilled water (38 mL) and concentrated HCl (6 mL, 72 mmol) at 0° C. was added sodium nitrite (1.99 g, 28.9 mmol) in H2O (10 mL). After 1.5 h, the mixture was allowed to warm to 25° C. and stirred for 1.5 h. Methyl disulfide (10.7 mL, 120 mmol) was added and the mixture heated to 70° C. for 18 h. The solvent was removed, in vacuo, to give an orange solid (16.7 g) that was used as is in the next reaction.

Aufarbeitung

  1. temperaturethe mixture heated to 70° C. for 18 h
  2. customThe solvent was removed, in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-54f1f3f8d62143288ddbbd602e2acee8
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07550629B2

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