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Diisopropylamine → 3-[(2-chlorophenyl)methyl]-2-propylthio-N-(diphenylmethylene)histidine ethyl ester

HRID 377226
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 377226
C(NC(C)C)(C)C.C([Li])CCC.[CH2:13]([O:15][C:16](=[O:32])[CH2:17][N:18]=[C:19]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:14].Cl.[Cl:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH2:41][N:42]1[C:46]([CH2:47]Cl)=[CH:45][N:44]=[C:43]1[S:49][CH2:50][CH2:51][CH3:52].[Cl-].[NH4+]>O1CCCC1.CN(C)C=O>[CH2:13]([O:15][C:16](=[O:32])[C@H:17]([CH2:47][C:46]1[N:42]([CH2:41][C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][C:35]=2[Cl:34])[C:43]([S:49][CH2:50][CH2:51][CH3:52])=[N:44][CH:45]=1)[N:18]=[C:19]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)[CH3:14]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 7912DiisopropylamineHCID 25517Ammonium ChlorideHCID 319508Ethyl 2-(diphenylmethyleneamino)acetateHCID 19351525HCID 19351525, VerbindungHCID 178418339Butyllithium

Produkt 1

HCID 537539713-[(2-chlorophenyl)methyl]-2-propylthio-N-(diphenylmethylene)histidine ethyl ester
Ausbeute 47,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of diisopropylamine (8.4 mL) in tetrahydrofuran (100 mL) was cooled to -78° C. under argon and a solution of n-butyl lithium (30 mL of 2.5 M in hexane) was added. The mixture was stirred at -78° C. for 30 minutes and at 0°C. for 10 minutes. After being recooled to -78° C., a solution of N-(diphenylmethylene)-glycine ethyl ester (Tetra. Lett., (1978), 2541, 4625) (15.4 g) in tetrahydrofuran (50 mL) was added, the mixture was stirred for 1 hour at -78° C. and a solution of 1-(2-chlorophenyl)methyl-5-chloromethyl-2-propylthio-1H-imidazole hydrochloride (9.4 g) in dry dimethylformamide (20 mL) was added. The mixture was then stirred at ambient temperature for 18 hours, poured into saturated ammonium chloride solution and the aqueous layer was extracted with methylene chloride. The organic extracts were washed with water, dried with magnesium sulfate concentrated and chromatographed over silica gel with 1% methanol in methylene chloride to afford 6.88 g of 3-[(2-chlorophenyl)methyl]-2-propylthio-N-(diphenylmethylene)histidine ethyl ester.

Aufarbeitung

  1. customAfter being recooled to -78° C.
  2. stirringthe mixture was stirred for 1 hour at -78° C.
  3. stirringThe mixture was then stirred at ambient temperature for 18 hours
  4. extractionthe aqueous layer was extracted with methylene chloride
  5. washThe organic extracts were washed with water
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated
  8. customchromatographed over silica gel with 1% methanol in methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-613b0f4815224a43b7582a4cedeb6f53
Quelldatensatz
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06025380

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