Sodium Carbonate → HCID 15296730, Verbindung

HRID 260077

Reaktionsgleichung

Reaktionsgleichung von HRID 260077
[C:1]1([CH:7]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:8]([N:10]2[CH:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([O:26][CH3:27])[C:16]=3[OH:25])[CH2:11]2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:34]([C:38]1[CH:45]=[CH:44][C:41]([CH2:42]Br)=[CH:40][CH:39]=1)([O:36][CH3:37])=[O:35].C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C>[C:34]([C:38]1[CH:45]=[CH:44][C:41]([CH2:42][O:25][C:16]2[C:15]([O:26][CH3:27])=[CH:14][CH:13]=[C:12]3[C:17]=2[CH2:18][CH:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[N:10]([C:8](=[O:9])[CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[CH2:11]3)=[CH:40][CH:39]=1)([O:36][CH3:37])=[O:35]

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 15296729(RS)-2-(Diphenylacetyl)-1,2,3,4-tetrahydro-5-hydroxy-6-methoxy-3-isoquinolinecarboxylic acid, ethyl ester

Produkt 1

HCID 15296730HCID 15296730, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 0.89 g (0.002 mole) of the compound from Example 31, 0.69 g (0.003 mole) of 4-carbomethoxybenzyl bromide (Aldrich), 5.0 g of powdered anhydrous sodium carbonate, and 5 mL of DMF is heated at reflux, with stirring, for 5 minutes. The cooled mixture is treated with 50 mL of ice water. The precipitated product is extracted into 150 mL of ether. The solution is dried (magnesium sulfate) and concentrated; wt. of amorphous solid 1.20 g; mass spectrum (CI) 594 (M+).

Aufarbeitung

  1. temperatureis heated
  2. temperatureat reflux
  3. extractionThe precipitated product is extracted into 150 mL of ether
  4. dry with materialThe solution is dried (magnesium sulfate)
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-c8cd1f6258aa436ab13b9ae27cffeffe
Quelldatensatz
uspto-grants-1996_06
Patentnummer
US05525614

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