Benzoic acid, 2-chloro-5-(chlorosulfonyl)- → HCID 20505867, Verbindung

HRID 355129

Reaktionsgleichung

Reaktionsgleichung von HRID 355129
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[NH:15]1[CH2:20][CH2:19][CH:18]([CH2:21][OH:22])[CH2:17][CH2:16]1>C(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11]([N:15]2[CH2:20][CH2:19][CH:18]([CH2:21][OH:22])[CH2:17][CH2:16]2)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

Komponenten

4

Edukt 2

HCID 67306Benzoic acid, 2-chloro-5-(chlorosulfonyl)-HCID 4207714-Piperidinemethanol

Produkt 1

HCID 20505867HCID 20505867, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2-Chloro-5-chlorosulfonylbenzoic acid (5.0 g.) is added to a solution of 4-piperidyl carbinol (6.9 g.) in 40 ml. of methylene chloride. The solution is refluxed for 2 hours, cooled to room temperature and stirred overnight. The solution is evaporated to dryness, the gummy residue dissolved in 1 N sodium hydroxide, and the alkaline solution extracted twice with ether. The aqueous solution is acidified with concentrated hydrochloric acid, and the precipitate recovered by filtration. Recrystallization from ethyl acetate yields crystals, m.p. 185°-187° C.

Aufarbeitung

  1. temperatureThe solution is refluxed for 2 hours
  2. customThe solution is evaporated to dryness
  3. dissolutionthe gummy residue dissolved in 1 N sodium hydroxide
  4. extractionthe alkaline solution extracted twice with ether
  5. filtrationthe precipitate recovered by filtration
  6. customRecrystallization from ethyl acetate
  7. customyields crystals, m.p. 185°-187° C.

Quellen und Nachweise

ORD-Eintrag
ord-37bfdf2cf16e4d66871ca50ca34985de
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04377521

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