Water → HCID 2797875, Verbindung

HRID 1164505Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1164505
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1.C(N(CC)CC)C.O>C(Cl)(Cl)Cl>[CH3:1][S:2]([NH:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)(=[O:4])=[O:3]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 832754-Pyridineethanamine

Produkt 1

HCID 2797875HCID 2797875, VerbindungAusbeute 23,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

Methanesulphonyl chloride (3.5 g.) was added slowly to 4-(2-aminoethyl)pyridine (3.6 g.) and triethylamine (3.0 g.) in chloroform (40 ml.). The temperature was maintained below 40° C. during the addition, after which the orange solution was left to stand at room temperature overnight. Water (50 ml.) was then added, the chloroform phase was separated, and the aqueous phase extracted with chloroform (100 ml.). The two chloroform solutions were combined, dried (MgSO4) and taken to dryness in vacuo to give a yellow oil which solidified immediately. This solid was crystallized from ethanol to yield white crystals of 4-(2-methanesulphonamidoethyl)pyridine (1.4 g.).

Aufarbeitung

  1. temperatureThe temperature was maintained below 40° C. during the addition
  2. waitafter which the orange solution was left
  3. customthe chloroform phase was separated
  4. extractionthe aqueous phase extracted with chloroform (100 ml.)
  5. dry with materialdried (MgSO4)
  6. customto give a yellow oil which
  7. customThis solid was crystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-780155ae895945a7860c0be2f63f9383
Quelldatensatz
uspto-grants-1983_01
Patentnummer
US04370328

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