Cesium carbonate → HCID 11540788, Verbindung

HRID 1437447Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1437447
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][CH2:14][CH2:15][CH2:16]Br)=[CH:9][C:8]=1[CH3:18])[CH3:2].[N:20]1[N:21]([C:29]2[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:30]=2[OH:36])[N:22]=[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=12.C([O-])([O-])=O.[Cs+].[Cs+]>CC#N>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][CH2:14][CH2:15][CH2:16][O:36][C:30]2[CH:31]=[CH:32][C:33]([Cl:35])=[CH:34][C:29]=2[N:21]2[N:22]=[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]3=[N:20]2)=[CH:9][C:8]=1[CH3:18])[CH3:2]

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 20446366HCID 20446366, VerbindungHCID 57941270HCID 57941270, Verbindung

Produkt 1

HCID 11540788HCID 11540788, VerbindungAusbeute 70,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture of [4-(3-bromo-propylsulfanyl)-2-methyl-phenoxy]-acetic acid ethyl ester (139 mg, 0.4 mmol) and 2-benzotriazole-2-yl-4-chloro-phenol (108 mg, 0.44 mmol) in MeCN (3 mL) was added Cs2CO3 (156 mg, 0.48 mmol). The mixture was stirred at room temperature for 4 hrs. The mixture was filtrated through Celite and washed with ethyl acetate. The solvent was evaporated and the residue was purified by flash chromatography on silica gel to give 145 mg of the desired ester.

Aufarbeitung

  1. filtrationThe mixture was filtrated through Celite
  2. washwashed with ethyl acetate
  3. customThe solvent was evaporated
  4. customthe residue was purified by flash chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-59b6a5b0cdaf432c9c342c000d18fb5f
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07622491B2

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