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ChemicalBook CAS DataBase List 6-BROMO-PHTHALAZINE

6-BROMO-PHTHALAZINE synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with hydrazine in ethanol;dichloromethane at 0; for 1 h;

Steps:

7.1 N-(4-Methyl-3-phthalazin-6-yl-phenyl)-3-trifluoromethyl-benzamide
Step 7.1: 6-Bromo-phthalazine A solution of 1.0 g (4.7 mmol) 4-bromo-benzene-1,2-dicarbaldehyde in 4 mL of ethanol and 4 ml of dichloromethane is added dropwise over 40 min at 0° C. and under nitrogen to a solution of hydrazine hydrate (0.684 mL, 14.1 mmol) in 4.7 mL of ethanol. The resulting suspension is stirred 1 h at 0° C. and then the solvent is evaporated. The crystalline material is stirred with 20 mL of toluene and the solvent is evaporated again. This procedure is repeated with dichloromerthane. At the end the product is dried at 60° C. under vacuum for 8 h to give the title compound as colorless crystals: m.p. 140-143° C., HPLC tR=1.49 min; ME-ES+: (M+H)+=210.9.

References:

Caravatti, Giorgio;Furet, Pascal;Imbach, Patricia;Martiny-Baron, Georg;Perez, Lawrence Blas;Sheng, Tao US2006/35897, 2006, A1 Location in patent:Page/Page column 22

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