Sodium Hydroxide → 3-Chloro-5-(3,5-dimethylpiperidinosulfonyl)benzoic Acid

HRID 1730606Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1730606
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([S:11](Cl)(=[O:13])=[O:12])[CH:10]=1)[C:5]([OH:7])=[O:6].Cl.[CH3:16][CH:17]1[CH2:22][CH:21]([CH3:23])[CH2:20][NH:19][CH2:18]1.[OH-].[Na+]>O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([S:11]([N:19]2[CH2:20][CH:21]([CH3:23])[CH2:22][CH:17]([CH3:16])[CH2:18]2)(=[O:13])=[O:12])[CH:10]=1)[C:5]([OH:7])=[O:6]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 38612753-Chloro-5-(chlorosulfonyl)benzoic acidHCID 22670446HCID 22670446, Verbindung

Produkt 1

HCID 205059493-Chloro-5-(3,5-dimethylpiperidinosulfonyl)benzoic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

3-Chloro-5-chlorosulfonylbenzoic acid (770 mg., 3 m moles) is added to a solution of 3,5-dimethylpiperidine hydrochloride in 30 ml. of water followed by the portionwise addition of 12 ml. of 1N sodium hydroxide solution with stirring. After 1.5 hrs. at room temperature the reaction mixture is filtered and the filtrate acidified with 12N hydrochloric acid.The product, 600 mg., m.p. 226°-231° C., is recrystallized from acetone-hexane, 390 mg., m.p. 232.5°-234° C.

Aufarbeitung

  1. filtrationat room temperature the reaction mixture is filtered
  2. custom, m.p. 226°-231° C., is recrystallized from acetone-hexane, 390 mg

Quellen und Nachweise

ORD-Eintrag
ord-228c33e414cc4408bc89b6cf49ee893a
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03992441

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