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    • 3. 发明授权
    • Asymmetric catalytic reduction of oxcarbazepine
    • 奥卡西平的不对称催化还原
    • US08288532B2
    • 2012-10-16
    • US11997104
    • 2006-04-21
    • David Alexander LearmonthGabriela Alexandra GrasaAntonio Zanotti-Gerosa
    • David Alexander LearmonthGabriela Alexandra GrasaAntonio Zanotti-Gerosa
    • C07D223/22
    • C07D223/28A61K31/55C07D223/22
    • A process for preparing (S)-(+)-10,11-dihydro-10-hydroxy-5H-dibenz/b,f/azepine-5-carboxamide or (R)-(−)-10,11-dihydro-10-hydroxy-5H-dibenz/b,f/azepine-5-carboxamide, by reduction of oxcarbazepine in the presence of a catalyst and a hydride source is disclosed. The catalyst is prepared from a combination of [RuX2(L)]2 wherein X is chlorine, bromine or iodine, and L is an aryl or aryl-aliphatic ligand, with a ligand of formula (A) or formula (B): wherein R1 is chosen from C1-6 alkoxy and C1-6 alkyl, n is a number from 0 to 5, and when n is a number from 2 to 5, R1 can be the same or different, and R2 is alkyl, substituted alkyl, aryl, substituted aryl, alkaryl or substituted alkaryl. The hydride source is either NR3R4R5 and formic acid, [R3R4R5NH][OOCH] and optionally formic acid, or [M][OOCH]x and formic acid, wherein R3, R4 and R5 are C1-6 alkyl, M is an alkali metal or alkaline earth metal and x is 1 or 2. A pH from 6.5 to 8 is maintained during the process.
    • 制备(S) - (+) - 10,11-二氢-10-羟基-5H-二苯并/ b,f /氮杂-5-甲酰胺或(R) - ( - ) - 10,11-二氢 - 公开了在催化剂和氢化物源存在下还原奥卡西平的方法,其中10-羟基-5H-二苯并/ b,f /吖庚因-5-甲酰胺。 催化剂由[RuX 2(L)] 2(其中X是氯,溴或碘)和L是芳基或芳基 - 脂族配体与式(A)或式(B)的配体的组合制备:其中 R 1选自C 1-6烷氧基和C 1-6烷基,n为0至5的数,当n为2至5的数时,R 1可相同或不同,并且R 2为烷基,取代的烷基, 芳基,取代的芳基,烷芳基或取代的烷芳基。 氢化物源是NR3R4R5和甲酸,[R3R4R5NH] [OOCH]和任选的甲酸或[M] [OOCH] x和甲酸,其中R3,R4和R5是C1-6烷基,M是碱金属 或碱土金属,x为1或2.在该过程中维持6.5至8的pH。