CAS: 69225-59-8; 3,3-Dimethyl-1,5-Dioxaspiro[5.5]Undecan-9-One

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N,N'-Bis(3,3-Dimethyl-1,5-Dioxaspiro<5.5>Undecan-9-Yliden)Hydrazin置于hof* Ch3Cn体系中,用 二氯甲烷 作为反应溶剂,化学反应 0.02H,以80%的收率获得产物3,3-二甲基-1,5-二氧杂螺[5.5]十一烷-9-酮
参考文献:一种新的有效脱保护嗪,和肟的方法.交换羰基中氧同位素的绝佳途径
标题:一种新的有效脱保护嗪,和肟的方法.交换羰基中氧同位素的绝佳途径
摘要:可以通过hof.ch 3 Cn在几秒钟内将hos.ch 3 Cn脱保护为相应的酮或醛,从而获得非常好的收率,从而可以保护作为嗪或其他cn衍生物的羰基.该反应还提供了一种非常有效的途径,可以用任何其他氧同位素(例如[18] O)取代大多数羰基的氧原子.
DOI:10.1016/j.Tetlet.2005.11.090

专利信息

专利号:US-2007129554-A1
优先权日:2005-10-24
标题 :Alpha functionalization of cyclic, ketalized ketones and products therefrom
发明人：HARRINGTON PETER J; KHATRI HIRALAL N; KHATRI SUDHA
权利人:HARRINGTON PETER J; KHATRI HIRALAL N; KHATRI SUDHA
摘要:Methodologies for the alpha-monohalogenation of acid sensitive ketones, especially cyclic, acid-sensitive, ketalized ketones. As one approach, the ketone is reacted with a halogen donor compound, e.g., N-chlorosuccinimide, in anhydrous, highly polar organic reagents such as dimethylformamide (DMF). As another monohalogenation approach, it has been observed that organic salts generated from amines and carboxylic acids catalyze the monohalogenation of ketalized ketone in reagents comprising alcohol solvent (methanol, ethanol, isopropanol, etc.). The monohalogenation is fast even at −5° C. The salt can be rapidly formed in situ from ingredients including amines and/or carboxylic acids without undue degradation of the acid sensitive ketal. Aryl ketones are monooxygenated using iodosylbenzene. This methodology is applied to monohalogenation of an acid sensitive monoketal ketone. The ability to prepare monohalogenated, acid sensitive ketones facilitates syntheses using halogenated, acid sensitive ketones. As just one example, facile synthesis of halogenated, acid sensitive ketones provides a new approach to synthesize the S-ketal-acid S-MBA (S-methylbenzylamine) salt useful as an intermediate in the manufacture of a glucokinase activator. As an overview of this scheme, a monohalogenated, cyclic, ketalized ketone is prepared using monohalogenation methodologies of the present invention. The halogenated compound is then subjected to a Favorskii rearrangement under conditions to provide the racemic acid counterpart of the desired chiral salt. The desired chiral salt is readily recovered in enantiomerically pure form from the racemic mixture.

专利号:US-4587351-A
优先权日:1984-04-18
标 题 :Synthesis of ketones with calcium hypochlorite
发明人：ATKINS RANDALL K; WEIGEL LELAND O
权利人:LILLY CO ELI
摘要:The present invention pertains to a process for preparing ketones employing a silica catalyzed oxidation of a secondary alcohol with calcium hypochlorite in acetonitrile.

专利号:US-4460604-A
优先权日:1976-06-03
标 题 :4-Amino-4-aryl-cyclohexanones
发明人：LEDNICER DANIEL
权利人:UPJOHN CO
摘要:A class of 4-amine-4-arylcyclohexanones, their ketals, and acid addition salts have been synthesized and found to be useful for relieving pain in animals. Their analgesic activity appears to be of high order, and in addition some exhibit narcotic antagonist activity that is useful in modifying the cardiovascular, respiratory, and behavioral depression caused by other analgesics. Several show mixed analgesic and narcotic antagonist activity. Preferred compounds of the class are 4-(m-hydroxyphenyl)-4-dimethylaminocyclohexanone ethylene ketal, and 4-(m-hydroxyphenyl)-4-(n-butylmethylamino)cyclohexanone ethylene ketal as free bases and as their hydrochloride salts. Processes for synthesis and intermediates are described. Unit dosage forms and therapeutic treatments are disclosed.