Potassium Carbonate → HCID 57597564, Verbindung

HRID 1786555Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1786555
Br[CH:2]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:15]([O:17][C:18]([C@@H:20]1[CH2:24][C@H:23]([NH:25][C:26](=[O:41])[CH2:27][CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:22][NH:21]1)=[O:19])[CH3:16].C([O-])([O-])=O.[K+].[K+]>CC(=O)CC>[CH2:15]([O:17][C:18]([C@@H:20]1[CH2:24][C@H:23]([NH:25][C:26](=[O:41])[CH2:27][CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH2:22][N:21]1[CH:2]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:19])[CH3:16]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 236603BromodiphenylmethaneHCID 57597565HCID 57597565, Verbindung

Produkt 1

HCID 57597564HCID 57597564, VerbindungAusbeute 57,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

To a solution of bromodiphenylmethane (0.4 g, 1.64 mmol) in butanone (10 ml) was added (2S,4S)-4-(3,3-diphenyl-propionylamino)-pyrrolidine-2-carboxylic acid ethyl ester (36) (0.6 g, 1.64 mmol), K2CO3 (0.23 g, 1.64 mmol) and KI (0.27 g, 1.64 mmol). The mixture was heated under reflux for 18 hours, and then filtered and the solvent was removed in vacuo. The residue was dissolved in CH2Cl2 (50 ml) and washed with water (10 ml). Drying over MgSO4 and removal of solvent under reduced pressure followed by column chromatography using Hex:EtOAc (1:1) gives 0.5 g the desired product.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residue was dissolved in CH2Cl2 (50 ml)
  6. washwashed with water (10 ml)
  7. dry with materialDrying over MgSO4 and removal of solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bac9ddbcb8d04a9bba676089661f1a08
Quelldatensatz
uspto-grants-2009_03
Patentnummer
US07507760B2

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