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ChemicalBook CAS DataBase List 7-chloro-1,3-dihydro-5-phenyl-2-oxo-2H-1,4-benzodiazepin-3-yl acetate

7-chloro-1,3-dihydro-5-phenyl-2-oxo-2H-1,4-benzodiazepin-3-yl acetate synthesis

5synthesis methods
-

Yield:1824-74-4 92.4%

Reaction Conditions:

with anhydrous Sodium acetate in N,N-dimethyl-formamide at 95 - 100; for 2 h;Reagent/catalyst;Solvent;Temperature;

Steps:

1-3; 1-4 Example 1

Add 30g of 7-chloro-2-oxo-5-phenyl-2,3-dihydro-1-H-1,4-benzodiazepine-4-oxide into the reaction flask successively,24ml acetic anhydride,24ml of dimethylformamide and 3g of anhydrous sodium acetate are heated to 95100 with stirring,The reaction was then incubated for 2 hours. Cool down to 0°C, add 12g water dropwise, and finish adding,Continue to stir at -50 for 0.5 hours, let stand for more than 2 hours, filter,Washed with water to obtain the crude oxazepam intermediate. The crude product was added to a mixed solvent of 90ml of ethanol and 30ml of water, beating and refining to obtain 31.8g of oxazepam intermediate,The HPLC purity was 99.4%, and the yield was 92.4%.

References:

CN113816913,2021,A Location in patent:Paragraph 0018; 0031; 0036-0049