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    • 4. 发明申请
    • ASYMMETRIC CATALYTIC REDUCTION OF OXCARBAZEPINE
    • 不对称催化还原氧化腈
    • WO2007012793A1
    • 2007-02-01
    • PCT/GB2006/001473
    • 2006-04-21
    • PORTELA & C.A., S.A.LEARMONTH, David, AlexanderGRASA, Gabriela, AlexandraZANOTTI-GEROSA, Antonio
    • LEARMONTH, David, AlexanderGRASA, Gabriela, AlexandraZANOTTI-GEROSA, Antonio
    • 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,l l-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 [RuX 2 (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 R 1 is chosen from C 1-6 alkoxy and C 1-6 alkyl, n is a number from 0 to 5, and when n is a number from 2 to 5, R 1 can be the same or different, and R 2 is alkyl, substituted alkyl, aryl, substituted aryl, alkaryl or substituted alkaryl. The hydride source is either NR 3 R 4 R 5 and formic acid, [R 3 R 4 R 5 NH][OOCH] and optionally formic acid, or [M][OOCH] x and formic acid, wherein R 3 , R 4 and R 5 are C 1-6 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 /吖庚因-5-甲酰胺或(R) - ( - ) - 10,11-二氢 公开了在催化剂和氢化物源的存在下还原奥卡西平的方法,将10-羟基-5H-二苯并/ b,f /吖庚因-5-甲酰胺。 催化剂由[RuX 2(L)] 2 N的组合制备,其中X是氯,溴或碘,L是芳基或芳基 - 脂族配体, 与式(A)或式(B)的配位体反应:其中R 1选自C 1-6烷氧基和C 1-6 - >烷基,n是0至5的数,当n是2至5的数时,R 1可以相同或不同,R 2是 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NR 3 S 4 R 5和甲酸,[R 3 S 3 R 5] 4 O 5 H] [OOCH]和任选的甲酸或[M] [OOCH] x X和甲酸,其中R 3, R 4,R 4和R 5是C 1-6烷基,M是碱金属或碱土金属,x是1 或2.在该过程中维持6.5至8的pH。