HCID 86756334, Verbindung → Sampatrilat

HRID 567943Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 567943
O.[C:2]([C@H:5]([CH2:27][NH:28][C:29](=[O:41])[C@H:30]([CH2:36][CH2:37][CH2:38][CH2:39][NH2:40])[NH:31][S:32]([CH3:35])(=[O:34])=[O:33])[CH2:6][C:7]1([C:12]([NH:14][C@H:15]([C:24]([OH:26])=[O:25])[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[O:13])[CH2:11][CH2:10][CH2:9][CH2:8]1)([OH:4])=[O:3]>O.CC(C)=O>[C:2]([C@H:5]([CH2:27][NH:28][C:29](=[O:41])[C@H:30]([CH2:36][CH2:37][CH2:38][CH2:39][NH2:40])[NH:31][S:32]([CH3:35])(=[O:34])=[O:33])[CH2:6][C:7]1([C:12]([NH:14][C@H:15]([C:24]([OH:26])=[O:25])[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[O:13])[CH2:11][CH2:10][CH2:9][CH2:8]1)([OH:4])=[O:3]

Komponenten

4

Edukt 1

HCID 86756334HCID 86756334, Verbindung

Produkt 1

HCID 6324648Sampatrilat

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

(S,S,S)-N-(1-[2-Carboxy-3-(N2-mesyllysylamino)propyl]-1-cyclopentylcarbonyl)tyrosine hydrate (the δ-form, see Preparation 2) (847.0 g) was dissolved in water (762 ml) and the solution diluted with acetone (1.0 l). This solution was added slowly to vigorously stirred acetone (18.05 l) at room temperature and a white solid precipitated. The mixture was stirred at room temperature for 18 hours, the solid was collected by filtration, washed with acetone and dried to give the title compound as a white solid (775 g), m.p. 179-181° C. Found: C,53.42; H,6.88; N,9.37; S,5.49. C26H40N4O9S requires: C,53.41; H,6.90; N,9.58; S,5.48%.

Aufarbeitung

  1. customPreparation 2) (847.0 g)
  2. customa white solid precipitated
  3. filtrationthe solid was collected by filtration
  4. washwashed with acetone
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2d8a21e2f32e4ae68eb74d02fae69bf1
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06180665B2

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