Triethylamine → 4-Amino-N-[1-((4-amino-3-nitro-phenyl)-methyl)-2-(4-methyl-piperidin-1-yl)-2-oxo-ethyl]-3,5-dichlorobenzenesulphonamide

HRID 274957Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 274957
[NH2:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][C@@H:7]([C:9]([N:11]2[CH2:16][CH2:15][CH:14]([CH3:17])[CH2:13][CH2:12]2)=[O:10])[NH2:8])=[CH:4][C:3]=1[N+:20]([O-:22])=[O:21].C(N(CC)CC)C.[NH2:30][C:31]1[C:36]([Cl:37])=[CH:35][C:34]([S:38](Cl)(=[O:40])=[O:39])=[CH:33][C:32]=1[Cl:42]>C(Cl)Cl>[NH2:30][C:31]1[C:36]([Cl:37])=[CH:35][C:34]([S:38]([NH:8][CH:7]([CH2:6][C:5]2[CH:18]=[CH:19][C:2]([NH2:1])=[C:3]([N+:20]([O-:22])=[O:21])[CH:4]=2)[C:9]([N:11]2[CH2:12][CH2:13][CH:14]([CH3:17])[CH2:15][CH2:16]2)=[O:10])(=[O:40])=[O:39])=[CH:33][C:32]=1[Cl:42]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 186592934-Amino-3-nitro-phenylalanyl-(4-methyl-piperidine)HCID 189759814-Amino-3,5-dichlorobenzene-1-sulfonyl chloride

Produkt 1

HCID 200890424-Amino-N-[1-((4-amino-3-nitro-phenyl)-methyl)-2-(4-methyl-piperidin-1-yl)-2-oxo-ethyl]-3,5-dichlorobenzenesulphonamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

3.06 g (10 mMol) of 4-amino-3-nitro-phenylalanyl-(4-methyl-piperidine) are dissolved in 100 ml of methylene chloride and combined with 2.8 ml (20 mMol) of triethylamine. Then at ambient temperature 3.1 g (12 mMol) of 4-amino-3,5-dichloro-benzenesulphonic acid chloride in 20 ml of methylene chloride is slowly added dropwise. After 2 hours the precipitate is suction filtered, washed with methylene chloride and dried at 70° C. For further purification the precipitate is suspended in 100 ml of ethanol, decocted and after cooling suction filtered again.

Aufarbeitung

  1. filtrationsuction filtered
  2. washwashed with methylene chloride
  3. customdried at 70° C
  4. customFor further purification the precipitate
  5. temperatureafter cooling suction
  6. filtrationfiltered again

Quellen und Nachweise

ORD-Eintrag
ord-cffdfd0cd4324365967dd6d75102a36f
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05391556

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