Pyridine → HCID 19775872, Verbindung

HRID 1613447

Reaktionsgleichung

Reaktionsgleichung von HRID 1613447
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][NH:9][C:10](=[O:14])[O:11][CH2:12][CH3:13].N1C=CC=CC=1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:1][S:2]([O:6][CH2:7][CH2:8][NH:9][C:10](=[O:14])[O:11][CH2:12][CH3:13])(=[O:4])=[O:3]

Komponenten

6

Edukt 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 223805ethyl N-(2-hydroxyethyl)carbamate

Produkt 1

HCID 19775872HCID 19775872, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

60 g of methanesulfonyl chloride are metered over approximately 30 minutes at 0° to +5° C. to a solution of 66.5 g of ethyl 2-hydroxyethylcarbamate, 43.5 g of pyridine and 1.9 g of 4-dimethylaminopyridine in 150 ml of methylene chloride, with stirring, and the mixture is stirred for 2 more hours at +5° C. and then for 16 hours at room temperature. The reaction mixture is filtered, the residue is washed with a small quantity of ethyl acetate, and the combined filtrates are washed with dilute hydrochloric acid and water. After the mixture has been dried over magnesium sulfate, the solvent mixture is removed completely by distillation in vacuo, which gives ethyl 2-methylsulfonyloxyethylcarbamate, nD20 1.4450.

Aufarbeitung

  1. stirringthe mixture is stirred for 2 more hours at +5° C.
  2. filtrationThe reaction mixture is filtered
  3. washthe residue is washed with a small quantity of ethyl acetate
  4. washthe combined filtrates are washed with dilute hydrochloric acid and water
  5. dry with materialAfter the mixture has been dried over magnesium sulfate
  6. customthe solvent mixture is removed completely by distillation in vacuo, which

Quellen und Nachweise

ORD-Eintrag
ord-d5c6d3b9d70e4c06980dc58cd703dd91
Quelldatensatz
uspto-grants-1993_03
Patentnummer
US05192803

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