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HCID 10604239, Verbindung → L 738167

HRID 399439
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 399439
[C:1]1([CH3:45])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C@@H:11]([CH2:15][NH:16][C:17]([C:19]2[CH:44]=[C:22]3[C:23](=[O:43])[N:24]([CH2:28][CH2:29][CH:30]4[CH2:35][CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH2:31]4)[CH2:25][CH2:26][CH2:27][N:21]3[N:20]=2)=[O:18])[C:12]([OH:14])=[O:13])(=[O:9])=[O:8])=[CH:3][CH:2]=1>C(Cl)Cl>[C:1]1([CH3:45])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C@@H:11]([CH2:15][NH:16][C:17]([C:19]2[CH:44]=[C:22]3[C:23](=[O:43])[N:24]([CH2:28][CH2:29][CH:30]4[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]4)[CH2:25][CH2:26][CH2:27][N:21]3[N:20]=2)=[O:18])[C:12]([OH:14])=[O:13])(=[O:8])=[O:9])=[CH:3][CH:2]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 10604239HCID 10604239, Verbindung

Produkt 1

HCID 153986L 738167

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

15-1 (7.42 g, 11.48 mmol) was placed in a 1L round bottom flask equipped with a magnetic stir bar. Methylene chloride was added and the reaction mixture was cooled to 0°-5°. Hydrogen chloride was bubbled through the suspension with stirring. After about 2 min. the solid went into solution, and soon afterward a second precipitate formed. After bubbling gas through the suspension for an additional 5 min. the reaction flask was warmed to room temperature. After 30 min. the contents of the reaction flask were concentrated. The resulting white solid was the hydrochloride salt of 15-2 and by HPLC analysis was of >99% purity.

Aufarbeitung

  1. customequipped with a magnetic stir bar
  2. temperaturethe reaction mixture was cooled to 0°-5°
  3. customHydrogen chloride was bubbled through the suspension
  4. customsoon afterward a second precipitate formed
  5. customAfter bubbling gas through the suspension for an additional 5 min. the reaction flask
  6. concentrationAfter 30 min. the contents of the reaction flask were concentrated

Quellen und Nachweise

ORD-Eintrag
ord-2c9ef2b2557140458a3b70a13b69bb82
Quelldatensatz
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05821241

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