Hydrochloric Acid → HCID 57731990, Verbindung

HRID 1808249

Reaktionsgleichung

Reaktionsgleichung von HRID 1808249
N[C:2]1[CH:22]=[CH:21][C:5]([C:6]([NH:8][CH2:9][C:10]([O:13][C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)([CH3:12])[CH3:11])=[O:7])=[CH:4][C:3]=1[F:23].N([O-])=O.[Na+].[S:28](=[O:30])=[O:29].[ClH:31]>O.CC(O)=O.O.O.[Cu](Cl)Cl>[F:23][C:3]1[CH:4]=[C:5]([C:6]([NH:8][CH2:9][C:10]([O:13][C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)([CH3:12])[CH3:11])=[O:7])[CH:21]=[CH:22][C:2]=1[S:28]([Cl:31])(=[O:30])=[O:29]

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 1119Sulfur DioxideHCID 23668193Sodium NitriteHCID 577322414-Amino-3-fluoro-N-[2-(4-fluorophenoxy)-2-methylpropyl]benzamide

Produkt 1

HCID 57731990HCID 57731990, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 61482Cupric chloride dihydrateKatalysatorHCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel3×

Versuchsvorschrift

4-Amino-3-fluoro-N-[2-(4-fluorophenoxy)-2-methylpropyl]benzamide (Preparation 94, 441 mg, 1.24 mmol) in 6 M of HCl in water (2 mL) was cooled at −5° C. Sodium nitrite (94.0 mg, 1.36 mmol) in water (0.5 mL, 30 mmol) was added slowly. After 20 minutes, sulfur dioxide in AcOH (8:25, sulfur dioxide:AcOH, 3 mL) and copper(II) chloride dihydrate (0.21 g, 1.2 mmol) were added to the reaction mixture. Vigorous gas evolution occurred. After 2 hours, the reaction was poured onto ice and water. The resulting solid was collected by filtration and washed with water and dried to afford a dark brown solid.

Aufarbeitung

  1. waitAfter 2 hours
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with water
  4. customdried
  5. customto afford a dark brown solid

Quellen und Nachweise

ORD-Eintrag
ord-73d4a73ba97341c6ba14a3e5d14c219f
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08357711B2

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