ChemicalBook CAS DataBase List Ophthazin Impurity 2

Ophthazin Impurity 2 synthesis

10synthesis methods

Product Name:Ophthazin Impurity 2
CAS Number:1044569-46-1
Molecular formula:C8H8N4
Molecular Weight:160.18

119-39-1
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1044569-46-1
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Yield:1044569-46-1 99%

Reaction Conditions:

with hydrazine at 0 - 25; for 24 h;Product distribution / selectivity;

Steps:

7.A Preparation of Hydralazine Base in the Absence of Organic Solvent

EXAMPLE 7A Preparation of Hydralazine Base in the Absence of Organic Solvent A 2 L, 3-necked, round-bottomed flask fitted with a temperature probe and condenser, and was charged 375 mL of hydrazine hydrate; the solution was then cooled to 0 to 5° C. About 75 g of 1-chlorophthalazine salt was added in portions at a rate to maintain the solution temperature at 0 to 5° C. After addition, the solution was stirred at 20 to 25° C. for about 24 hrs. The reaction mixture was then cooled to 0 to 5° C. and 150 mL of methanol was added, the solution stirred for 3 hrs, and the resulting solid material was filtered, washed with 150 mL of cold methanol, and dried under vacuum at 35° C. Yield 99%.

References:

US2007/129546,2007,A1 Location in patent:Page/Page column 5