HCID 178477443, Verbindung → HCID 178477444, Verbindung

HRID 329002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 329002
[N:1]#[N:2].C([O:7][C:8](=[O:44])[CH2:9][N:10]([C:16](=[O:43])[C@H:17]([CH2:36][CH2:37][CH2:38][NH:39][C:40](=[NH:42])[NH2:41])[NH:18][S:19]([C:22]1[CH:31]=[CH:30][C:29]2[C:24](=[CH:25][C:26]([O:34][CH3:35])=[C:27]([O:32][CH3:33])[CH:28]=2)[CH:23]=1)(=[O:21])=[O:20])[CH2:11][CH2:12][S:13][CH2:14][CH3:15])(C)(C)C>FC(F)(F)C(O)=O>[N:1]#[N:2].[CH3:33][O:32][C:27]1[CH:28]=[C:29]2[C:24](=[CH:25][C:26]=1[O:34][CH3:35])[CH:23]=[C:22]([S:19]([NH:18][C@H:17]([C:16]([N:10]([CH2:11][CH2:12][S:13][CH2:14][CH3:15])[CH2:9][C:8]([OH:44])=[O:7])=[O:43])[CH2:36][CH2:37][CH2:38][NH:39][C:40](=[NH:41])[NH2:42])(=[O:21])=[O:20])[CH:31]=[CH:30]2

Komponenten

3

Edukt 1

HCID 178477443HCID 178477443, Verbindung

Produkt 1

HCID 178477444HCID 178477444, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

A solution of 5.0 g of N2 -(6,7-dimethoxy-2-naphthalenesulfonyl)-L-arginyl-N-(2-ethylthioethyl)glycine tert-butyl ester in 10 ml of trifluoroacetic acid was stirred for 5 hours at room temperature. At the end of this period, the reaction mixture was evaporated to dryness. The residue was washed several times with dry diethyl ether and chromatographed on 80 ml of Daiaion SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited) packed in water, washed with water and eluted with ethanol-H2O-NH4OH (5:4:1).

Aufarbeitung

  1. customAt the end of this period, the reaction mixture was evaporated to dryness
  2. washThe residue was washed several times with dry diethyl ether
  3. customchromatographed on 80 ml of Daiaion SK 102 ion exchange resin (200-300 mesh, H+ form, manufactured by Mitsubishi Chemical Industries Limited)
  4. washwashed with water
  5. washeluted with ethanol-H2O-NH4OH (5:4:1)

Quellen und Nachweise

ORD-Eintrag
ord-0b72bac40efa444eac47e69c5fc30de4
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04018913

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