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ChemicalBook CAS DataBase List 10-Methoxycarbamazepine

10-Methoxycarbamazepine synthesis

12synthesis methods
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Yield: 85%

Reaction Conditions:

Stage #1:10-methoxy-5H-dibenzo[b,f]azepine;bis(trichloromethyl) carbonate with triethylamine in toluene at 10 - 15; for 6 h;
Stage #2: with ammonia in water;toluene at 20; for 1 h;

Steps:

1.a
) A solution of 66.9 g (0.3 mols) of 10-methoxy-iminostilbene and 34.92 g (0.34 mols) of triethylamine in 800 ml of toluene is gradually added, during 6 hours and at a temperature of 10-15°C, with a solution of 32.67 g (0.11 mols) of triphosgene in 300 ml of toluene. After completion of the reaction (disappearance of methoxy-iminostilbene) 200 ml of 30% aqueous ammonia are added gradually, vigorously stirring at room temperature for some hours. After that, the phases are separated, the toluene phase is washed with water and evaporated to dryness under reduced pressure. Yield: 69.0 g (85% on theoretical) of 10-methoxy-N-aminocarbonyl-iminostilbene (V) of purity higher than 95%.

References:

Milanese, Alberto EP1600443, 2005, A1 Location in patent:Page/Page column 8

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