HCID 86755658, Verbindung → HCID 86755659, Verbindung

HRID 1871995Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1871995
[CH2:1]([C:3]1[CH:50]=[CH:49][C:6]2[CH:7]([C:17]3[C:18]([S:47]C)=[N:19][C:20](=[O:46])[N:21]([C:23]4[CH:28]=[CH:27][N:26]=[C:25]([N:29]([CH3:45])[CH2:30][C:31]([NH:33][C:34]5[S:35][CH:36]=[C:37]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])[N:38]=5)=[O:32])[N:24]=4)[CH:22]=3)[C:8]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:9]=3[CH:10]=[CH:11][C:5]=2[CH:4]=1)[CH3:2]>N1C=CC=CC=1.C(N(CC)CC)C>[CH2:1]([C:3]1[CH:50]=[CH:49][C:6]2[CH:7]([C:17]3[C:18](=[S:47])[NH:19][C:20](=[O:46])[N:21]([C:23]4[CH:28]=[CH:27][N:26]=[C:25]([N:29]([CH3:45])[CH2:30][C:31]([NH:33][C:34]5[S:35][CH:36]=[C:37]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])[N:38]=5)=[O:32])[N:24]=4)[CH:22]=3)[C:8]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:9]=3[CH:10]=[CH:11][C:5]=2[CH:4]=1)[CH3:2]

Komponenten

4

Edukt 1

HCID 86755658HCID 86755658, Verbindung

Produkt 1

HCID 86755659HCID 86755659, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

The product from step (v) (0.61 g) was dissolved in dry pyridine (20 ml) and triethylamine (1.0 ml). Hydrogen sulphide gas was slowly bubbled through the solution for 15 minutes. The solvents were evaporated under reduced pressure and the residue azeotroped twice with toluene. The residue was purified by chromatography eluting with ethyl acetate in toluene. Yield 0.41 g.

Aufarbeitung

  1. customHydrogen sulphide gas was slowly bubbled through the solution for 15 minutes
  2. customThe solvents were evaporated under reduced pressure
  3. customthe residue azeotroped twice with toluene
  4. customThe residue was purified by chromatography
  5. washeluting with ethyl acetate in toluene

Quellen und Nachweise

ORD-Eintrag
ord-9b192823e3be4dffaac6af1fb1edc8a0
Quelldatensatz
uspto-grants-2000_08
Patentnummer
US06107297

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