Triethylamine → HCID 178428636, Verbindung

HRID 274959Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 274959
[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]([NH2:21])[C:12]([N:14]3[CH2:19][CH2:18][CH:17]([CH3:20])[CH2:16][CH2:15]3)=[O:13])=[CH:9][C:4]=2[N:3]=[CH:2]1.C(N(CC)CC)C.[CH3:29][N:30]1[C:42]2[CH2:41][CH2:40][CH2:39][CH2:38][C:37]=2[C:36]2[C:31]1=[CH:32][CH:33]=[C:34]([S:43](Cl)(=[O:45])=[O:44])[CH:35]=2>C(Cl)(Cl)Cl>[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]([NH:21][S:43]([C:34]3[CH:35]=[C:36]4[C:31](=[CH:32][CH:33]=3)[N:30]([CH3:29])[C:42]3[CH2:41][CH2:40][CH2:39][CH2:38][C:37]4=3)(=[O:44])=[O:45])[C:12]([N:14]3[CH2:19][CH2:18][CH:17]([CH3:20])[CH2:16][CH2:15]3)=[O:13])=[CH:9][C:4]=2[N:3]=[CH:2]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 218061079-Methyl-1,2,3,4-tetrahydro-carbazol-6-sulphonic acid chlorideHCID 178428665HCID 178428665, Verbindung

Produkt 1

HCID 178428636HCID 178428636, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

To a solution of 1 g (0.0034 Mol) of 1-(1H-benzimidazol-5-yl-methyl)-2-(4-methyl-piperidin-1-yl)-2-oxoethylamine and 1.1 g (0.011 Mol) of triethylamine in 30 ml of chloroform are added dropwise, at ambient temperature and with stirring, 0.96 g (0.0034 Mol) of 9-methyl-1,2,3,4-tetrahydro-carbazol-6-sulphonic acid chloride dissolved in 10 ml of chloroform. After 12 hours' stirring the mixture is evaporated down in vacuo and the residue obtained is chromatographed over a silica gel column (eluant: ethyl acetate/methanol=9:1). The eluate having an Rf value of 0.3 is collected and evaporated down in vacuo.

Aufarbeitung

  1. stirringAfter 12 hours' stirring the mixture
  2. customis evaporated down in vacuo
  3. customthe residue obtained
  4. customis chromatographed over a silica gel column (eluant: ethyl acetate/methanol=9:1)
  5. customis collected
  6. customevaporated down in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-380a404e2f034ca6b2b6f1c617f70f41
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05391556

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