StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

HCID 57355799, Verbindung → Phthalimide

HRID 481035
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 481035
[N-]=C=S.N1CCC(N2C3C=CC=CC=3N(CCC[N:22]3[C:26](=[O:27])[C:25]4=[CH:28][CH:29]=[CH:30][CH:31]=[C:24]4[C:23]3=[O:32])C2=O)CC1>C(Cl)Cl.O>[C:26]1(=[O:27])[NH:22][C:23](=[O:32])[C:24]2=[CH:31][CH:30]=[CH:29][CH:28]=[C:25]12
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 57355799HCID 57355799, VerbindungHCID 178418790HCID 178418790, Verbindung

Produkt 1

HCID 6809Phthalimide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Di(2-pyridyl)thionocarbonate (0.286 g, 1.2 mM) was added to a cold (0° C.) solution of 1,1-di(p-anisyl)methyl amine (0.3 g, 1.2 mM) and triethylamine (0.17 ml) in methylene chloride (10 ml). The resulting mixture was slowly warmed up to RT over a 4 hour period then stirred at RT for additional 1 hour to provide the 1,1-di(p-anisyl)methyl isothiocyanate. The prepared isothiocyanate was added to Compound 53 (0.94 g, 0.43 mM), prepared in Example 53, dissolved in methylene chloride (10 ml). The mixture was stirred at RT overnight, diluted with water (20 ml) and the layers were separated. The aqueous layer was again extracted with methylene chloride (2×20 ml). The combined CH2Cl2 extracts were dried over MgSO4, evaporated in vacuo and chromatoraphed (EM silica gel 60, 10% EtOAc in CH2Cl2) to give the pthalimide intermediate. This intermediate, substituted for Compound 54, was treated as described in Example 55 to give the HCl salt of the product. m/z (MH+) 560

Aufarbeitung

  1. customprepared in Example 53
  2. customthe layers were separated
  3. extractionThe aqueous layer was again extracted with methylene chloride (2×20 ml)
  4. dry with materialThe combined CH2Cl2 extracts were dried over MgSO4
  5. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0a070f92f1e54b2092c17ab56acf1be1
Quelldatensatz
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06653478B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion