申请人:Great Lakes Chemical (Europe) GmbH
公开号:US06444848B1
公开(公告)日:2002-09-03
Process for the preparation of symmetrical diacylhydrazines having general formula (I): R1—CO—NH—NH—CO—R1 wherein R1 represents a linear or branched C1-C18 alkyl group; a linear or branched C2-C8 alkoxyalkyl group; a C2-C8 cyanoalkyl group; a C5-C8 cycloalkyl group, said cycloalkyl group optionally containing a heteroatom selected from oxygen, nitrogen and sulfur; a C6-C18 aryl group; a C7C20 arylalkyl group or alkylaryl group, said arylalkyl or alkylaryl groups optionally substituted with one or more hydroxyl groups, or with one or more linear or branched C1-C8 alkoxyl groups; comprising: (a) reacting an ester of a carboxylic acid having general formula (II): R1—CO—OR2 wherein R1 has the same meanings defined above and R2 represents a linear or branched C1-C18 alkyl group, with hydrazine, in its pure or hydrated state, obtaining a monoacylhydrazine having general formula (III): R1—CO—NH—NH2; (b) reacting the monoacylhydrazine having general formula (III) obtained in step (a), with a &bgr;-ketoester having general formula (IV): R3—CO—CH2—COOR4 wherein R3 represents a linear or branched C1-C18 alkyl group, or a C6-C18 aryl group and R4 represents a linear or branched C1-C18 alkyl group, obtaining the desired symmetrical diacylhydrazine having general formula (I).
制备具有通式(I)的对称二酰肼的过程如下:其中R1代表线性或支链C1-C18烷基;线性或支链C2-C8烷氧基烷基;C2-C8氰基烷基;C5-C8环烷基,所述环烷基可以选择氧、氮和硫作为杂原子;C6-C18芳基;C7-C20芳基烷基或烷基芳基,所述芳基烷基或烷基芳基可以选择一个或多个羟基或一个或多个线性或支链C1-C8烷氧基进行取代;包括以下步骤:(a)将具有通式(II)的羧酸酯与纯态或水合态的肼反应,得到具有通式(III)的单酰肼:R1—CO—NH—NH2;(b)将步骤(a)中获得的具有通式(III)的单酰肼与具有通式(IV)的β-酮酯反应:R3—CO—CH2—COOR4,其中R3代表线性或支链C1-C18烷基或C6-C18芳基,R4代表线性或支链C1-C18烷基,得到所需的具有通式(I)的对称二酰肼。