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    • 7. 发明授权
    • PROCESS FOR PREPARATION OF HYDRAZIDES
    • 用于生产酰肼
    • EP0874806B1
    • 2001-10-31
    • EP96942936.4
    • 1996-12-19
    • SCHERING CORPORATION
    • LEONG, WilliamSMITH, Lyman
    • C07C241/04
    • C07C241/04Y02P20/55C07C243/28
    • A process for producing a hydrazide of formula (1.0) is disclosed. The process comprises reacting a hydrazone of formula (2.0) or (2.1), wherein said hydrazone is in toluene, with a mixture of Grignard reagents, wherein said Grignard reagents are in a suitable organic solvent; wherein: (A) Z is a suitable carbonyl protecting group; (B) R is a suitable -OH protecting group; (C) R is selected from: H, a non-enolizable alkyl, a non-enolizable substituted alkyl, aryl, substituted aryl, -S-aryl, -S-(substituted aryl), -S-alkyl, -S-(substituted alkyl), alkoxy, substituted alkoxy, aryloxy, or substituted aryloxy; (D) said mixture of Grignard reagents comprises R MgX in admixture with R MgX; (E) R is a suitable alkyl, substituted alkyl, alkenyl, alkynyl, aryl, substituted aryl, or aralkyl group capable of adding to the -C=N group of the hydrazone to produce the hydrazide; (F) R is a suitable alkyl, substituted alkyl, aryl or substituted aryl group that is more sterically hindered than said R group; (G) X is independently selected from Cl, Br or I for each Grignard reagent; (H) when said hydrazone is a compound of formula (2.0) then the reaction is conducted at a temperature of about +30 to about -40 DEG C; and (I) when said hydrazone is a compound of formula (2.1) then the reaction is conducted at a temperature of about +40 to about -20 DEG C.