Ethanol → Benzamide,4-amino-n-(butylsulfonyl)-3-[[(2,4-dichlorophenyl)methyl]amino]-

HRID 276081Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 276081
[CH2:1]([S:5]([NH:8][C:9](=[O:29])[C:10]1[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[C:12]([NH:19][CH2:20][C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=2[Cl:28])[CH:11]=1)(=[O:7])=[O:6])[CH2:2][CH2:3][CH3:4].S(S([O-])=O)([O-])=O.[Na+].[Na+].C(O)C.O1CCCC1>O>[CH2:1]([S:5]([NH:8][C:9](=[O:29])[C:10]1[CH:15]=[CH:14][C:13]([NH2:16])=[C:12]([NH:19][CH2:20][C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=2[Cl:28])[CH:11]=1)(=[O:6])=[O:7])[CH2:2][CH2:3][CH3:4]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 8028TetrahydrofuranHCID 24489Sodium DithioniteHCID 18315434N-1-butanesulfonyl-3-(2,4-dichlorobenzylamino)-4-nitrobenzamide

Produkt 1

HCID 18315556Benzamide,4-amino-n-(butylsulfonyl)-3-[[(2,4-dichlorophenyl)methyl]amino]-Ausbeute 46,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

N-1-butanesulfonyl-3-(2,4-dichlorobenzylamino)-4-nitrobenzamide (0.505 g) was added to a mixture of 1.32 g of sodium hydrosulfite, 1 ml of ethanol, 1 ml of tetrahydrofuran and 1 ml of water at room temperature. The mixture was heat-refluxed for 40 minutes. The solvent was distilled off under reduced pressure, and water was added to the residue. The solid material precipitated was collected, and was dried. Further, the resulting material was washed with a mixed solution of 10 ml of methanol and 3 ml of water, and was dried to give 0.220 g of N-1-butanesulfonyl-4-amino-3-(2,4-dichlorobenzylamino)benzamide.

Aufarbeitung

  1. temperatureThe mixture was heat-refluxed for 40 minutes
  2. distillationThe solvent was distilled off under reduced pressure, and water
  3. additionwas added to the residue
  4. customThe solid material precipitated
  5. customwas collected
  6. customwas dried
  7. washFurther, the resulting material was washed with a mixed solution of 10 ml of methanol and 3 ml of water
  8. customwas dried

Quellen und Nachweise

ORD-Eintrag
ord-e3e7857f29904ffcaba848683c04b077
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06352985B1

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