Trimethyl orthoformate → Methyl 10-methoxy-5H-dibenz[b,f]azepine-5-carboxylate
Reaktionsgleichung
[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[CH2:8][C:7]2[CH:17]=[CH:18][CH:19]=[CH:20][C:6]1=2)=[O:4].[CH:21](OC)(OC)OC>CO.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9]([O:16][CH3:21])=[CH:8][C:7]2[CH:17]=[CH:18][CH:19]=[CH:20][C:6]1=2)=[O:4]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
A suspension of 10-oxo-10,11-dihydro-dibenzo[b,f]azepine-5-carboxylic acid methyl ester (15 g, 56 mmol) in methanol (75 ml) is heated to 60° C. and a catalytic amount of p-toluene sulfonic acid (0.213 g, 1.1 mmol) is added. After addition of trimethyl ortho-formate (6.25 g, 58.9 mmol) the solution is stirred at 60–70° C. for 4 hours. During this reaction the product precipitates as white crystals. The mixture is cooled to room temperature, filtered and dried to yield 15.5 g of pure title compound (98%).
Aufarbeitung
- customDuring this reaction the product
- customprecipitates as white crystals
- temperatureThe mixture is cooled to room temperature
- filtrationfiltered
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-f8483d1ab42b487c926effb172eaf081
- Quelldatensatz
- uspto-grants-2006_09
- Patentnummer
- US07112673B2
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