Dibutylamine → HCID 20505824, Verbindung

HRID 1703716Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1703716
[CH2:1]([NH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[Cl:10][C:11]1[C:19]([S:20](Cl)(=[O:22])=[O:21])=[CH:18][C:14]([C:15]([OH:17])=[O:16])=[CH:13][CH:12]=1>C(Cl)Cl>[Cl:10][C:11]1[C:19]([S:20](=[O:22])(=[O:21])[N:5]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:1][CH2:2][CH2:3][CH3:4])=[CH:18][C:14]([C:15]([OH:17])=[O:16])=[CH:13][CH:12]=1

Komponenten

4

Edukt 2

HCID 8148DibutylamineHCID 756134-Chloro-3-(chlorosulphonyl)benzoic acid

Produkt 1

HCID 20505824HCID 20505824, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 3.9 g. (0.03 mole) of di-n-butylamine in 15 ml. of methylene chloride is added 2.5 g. (0.01 mole) of 4-chloro-5-chlorosulfonylbenzoic acid (J. Pharm. Pharmacol., 683 (1962), and the resulting reaction mixture allowed to stir at room temperature for 3 hrs. The solvent is removed under reduced pressure and the residue partitioned between 1N sodium hydroxide and diethyl ether. The aqueous phase is separated, acidified with 12N hydrochloric acid and the precipitated solid filtered and dried, 3.0 g., m.p. 93°-96° C. Recrystallization from ether-hexane provides the pure product, 2.5 g., m.p. 94.5°-96.5° C.

Aufarbeitung

  1. custom, 683 (1962), and the resulting reaction mixture
  2. customThe solvent is removed under reduced pressure
  3. customthe residue partitioned between 1N sodium hydroxide and diethyl ether
  4. customThe aqueous phase is separated
  5. filtrationthe precipitated solid filtered
  6. customdried
  7. customRecrystallization from ether-hexane
  8. customprovides the pure product, 2.5 g

Quellen und Nachweise

ORD-Eintrag
ord-9be74d7c051a441d88912fa99628712c
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04124590

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