ChemicalBook CAS DataBase List 8-chloro-1-phenyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione

8-chloro-1-phenyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione synthesis

12synthesis methods

Product Name:8-chloro-1-phenyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione
CAS Number:22316-55-8
Molecular formula:C15H11ClN2O2
Molecular Weight:286.71

68406-47-3
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8-chloro-1-phenyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione

22316-55-8
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$65.00/1mg

Yield: 89.5%

Reaction Conditions:

with aluminum (III) chloride;triethylamine in tetrahydrofuran at 15 - 20; for 4 h;Autoclave;Reagent/catalyst;Concentration;

Steps:

3.b B. Preparation of intermediate III
Malonic acid diethyl ester 257g (1.61 µM), three aluminum chloride 215g (1.61 µM) of the eyes of the drying in the reactor, stirring at the room temperature to clarify; intermediate II 328g (1.5 µM), tetrahydrofuran 2400 ml and triethylamine 472g (4.66 µM) after mixing, into the above clear solution, temperature control in the 15 - 20 °C, stirring 4h, identification of the end point of the reaction (developing solvent: dichloromethane - petroleum ether=4:1, sample in accordance with the quenching method after extraction), the completion of the reaction, into the 1N sodium hydroxide solution with 210 ml, filtering out solid, dichloromethane is used for water 300 ml × 2 extraction, the combined organic layer, anhydrous sodium sulfate drying, filtering to remove the drying agent, the filtrate is concentrated to dry, the residue for recrystallization to obtain the proper amount of ethanol 385g (1.343 µM) intermediates III, the yield is 89.5%.

References:

Anhui Yixin Ming Pharmaceutical Technology Co., Ltd.;Xu, Kui;Wang, Yali;Ceng, Fei CN106243050, 2016, A Location in patent:Paragraph 0017; 0021; 0025

22316-45-6 Synthesis