Hydrochloric Acid → HCID 14234265, Verbindung

HRID 1194756Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1194756
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)(=[O:11])=[O:10])=[CH:4][CH:3]=1.[N:20]([O-])=O.[Na+].[ClH:24]>O>[ClH:24].[NH:1]([C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH2:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)(=[O:11])=[O:10])=[CH:4][CH:3]=1)[NH2:20]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 132861021-(4-Aminophenyl)-N-benzylmethanesulfonamideHCID 23668193Sodium Nitrite

Produkt 1

HCID 14234265HCID 14234265, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A thick suspension of the product of stage (b) (3.68 g) in conc. hydrochloric acid (50 ml) was stirred at -5° whilst a solution of sodium nitrite (0.9 g) in water (10 ml) was added dropwise so that temperature did not exceed 0°. Stirring was continued for 30 min. The resulting suspension was filtered to remove starting material and the filtrate added in a few portions to a solution of stannous chloride dihydrate (13.5 g) in hydrochloric acid (15 ml) at -20° and warmed to ambient temperature. The solid that separated was filtered off and recrystallised from hot methanol (100 ml) to give the title compound as white plates (0.39 g) m.p. 192°-193°. The mother liquors afforded a second crop (0.52 g).

Aufarbeitung

  1. additionwas added dropwise so that temperature
  2. customdid not exceed 0°
  3. filtrationThe resulting suspension was filtered
  4. customto remove
  5. additionthe filtrate added in a few portions to a solution of stannous chloride dihydrate (13.5 g) in hydrochloric acid (15 ml) at -20°
  6. customThe solid that separated
  7. filtrationwas filtered off
  8. customrecrystallised from hot methanol (100 ml)

Quellen und Nachweise

ORD-Eintrag
ord-c180ee72505c4f44b9b7aa32ef48f8e4
Quelldatensatz
uspto-grants-1989_03
Patentnummer
US04816470

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