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ChemicalBook CAS DataBase List 1,4-dibromophthalazine

1,4-dibromophthalazine synthesis

4synthesis methods
-

Yield: 93%

Reaction Conditions:

with phosphorus pentabromide at 140;Sealed tube;

Steps:

4
Preparation 41,4-DibromophthalazineCharge a pressure tube with phosphorus pentabromide (24.5 g, 54 1 mmol) and 2,3-dihydro-phthalazine-1,4-dione (5.00 g, 30.8 mmol). Seal the tube and heat at 140° C. for 6-7 h. Allow to cool overnight. Carefully open the tube due to pressure. Chisel out the solid and pour into ice water. Allow to stir in ice water and collect the resulting solid by vacuum filtration. Dry in a vacuum oven to obtain the final product (8.31 g, 93%). ES/MS (79Br, 81Br) m/z 288.8 (M+). Ref.: Can. J. Chem. 1965, 43, 2708.

References:

ELI LILLY AND COMPANY US2010/324048, 2010, A1 Location in patent:Page/Page column 4