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ChemicalBook CAS DataBase List 1H-1,4-Diazepine, hexahydro-1-methyl-4-(phenylmethyl)-

1H-1,4-Diazepine, hexahydro-1-methyl-4-(phenylmethyl)- synthesis

4synthesis methods
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Yield:59039-76-8 82.5%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 80; for 3 h;Reagent/catalyst;

Steps:

1; 2

Weigh N-benzyl homopiperazine (12.08g, 63.6mmol), and measure 60ml of N,N-dimethylformamide into the reaction flask, add potassium carbonate (26.37g, 190.8mmol), then weigh Methyl iodide (18.05g, 127.2mmol) was slowly added dropwise to the reaction solution, the temperature was raised to 80°C, kept stirring for 3h, and the reaction was monitored by TLC. After the reaction was completed, it was concentrated to dryness under reduced pressure. The ethyl ester was concentrated to dryness, and 75 ml of methanol was added for recrystallization to obtain 10.72 g of the product with a yield of 82.5%.

References:

CN114957163,2022,A Location in patent:Paragraph 0011; 0043; 0047; 0049; 0053