Ethylamine hydrochloride → 3-chloro-N-methylpropane-1-sulfonamide

HRID 1060833

Reaktionsgleichung

Reaktionsgleichung von HRID 1060833
[Cl:1][CH2:2][CH2:3][CH2:4][S:5](Cl)(=[O:7])=[O:6].Cl.[CH2:10]([NH2:12])C.C(=O)([O-])[O-].[K+].[K+]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(OCC)(=O)C>[CH3:10][NH:12][S:5]([CH2:4][CH2:3][CH2:2][Cl:1])(=[O:7])=[O:6]

Komponenten

6

Versuchsvorschrift

3-Chloropropylsulfonyl chloride 1 (16.8 g, 94.9 mmol), ethylamine hydrochloride (13.5 g, 200 mmol), and potassium carbonate (27.6 g, 200 mmol) were sequentially added to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg) to the mixture, the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica2 gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.

Aufarbeitung

  1. dry with materialdried over anhydrous sodium sulfate
  2. filtrationThe mixture was filtered through a small amount of silica2 gel
  3. concentrationthe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-1dc486a91e0940dfbce95d7559656c2a
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06525081B1

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