Dichloromethane → 2-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamide

HRID 68998

Reaktionsgleichung

Reaktionsgleichung von HRID 68998
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10](Cl)(=[O:12])=[O:11])([O-:3])=[O:2].ClCCl.[NH2:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.C(N(CC)CC)C>O>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1)(=[O:12])=[O:11])([O-:3])=[O:2]

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 8540512-(Pyridin-3-yl)ethan-1-amine

Produkt 1

HCID 465565342-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamideAusbeute 32,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-Nitrobenzene sulfonyl chloride (11.64 g) was added to a dichloromethane solution (100 ml) of 3-(2-aminoethyl)pyridine (6.11 g) and triethylamine (9 ml) at 0° C. The mixture was stirred at room temperature for 2 hours. Water was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure. The residue was crystallized from ethyl acetate to give the title compound (5.06 g) as a yellow powder.

Aufarbeitung

  1. extractionfollowed by extraction with dichloromethane
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure
  3. customThe residue was crystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c3ccd1da4a8f4ca2bfbf69713a3fb167
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822453B2

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