Preparation of racemic cis 8-benzyl-2,8-diazabicyclo[4,3,0]nonane
A diazabicyclic and racemic technology, which is applied in the field of preparation of pharmaceutical intermediates, can solve the problems of low reaction selectivity, low catalytic efficiency, and affecting product purity, so as to improve catalytic efficiency, selectivity and Sufficiency of reaction, effect of improving purity
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Embodiment 1
[0028] The preparation process of racemic cis 8-benzyl-2,8-diazabicyclo[4,3,0]nonane comprises the following steps:
[0029] Step S1: preparing an attachment carrier: immersing the solid carrier into a roughening solution to prepare an attachment carrier, the roughening solution being sodium hydroxide solution or sodium bifluoride solution;
[0030] Step S2: preparing a platinum dehydrogenation catalyst: using an impregnation method to load noble metal platinum on a silica solid support by impregnating into an impregnating solution containing noble metal ions, in parts by weight, the impregnating solution includes chloroplatinic acid 30 1 part, 1 part of rice furoic acid, 1 part of dichlorophenyl imidazole dioxolane, the load on the solid carrier is 0.1% of the weight of the solid carrier;
[0031] Step S3: Dehydrogenation reaction of piperidine ring: (R,R)-8-benzyl-2,8-diazabicyclo[4,3,0]nonane obtained by optical resolution and platinum dehydrogenation catalyst At a reactio...
Embodiment 2
[0034] The preparation process of racemic cis 8-benzyl-2,8-diazabicyclo[4,3,0]nonane comprises the following steps:
[0035] Step S1: preparing an attachment carrier: immersing the solid carrier into a roughening solution to prepare an attachment carrier, the roughening solution being sodium hydroxide solution or sodium bifluoride solution;
[0036] Step S2: preparing a platinum dehydrogenation catalyst: the noble metal platinum is supported on the porous alumina solid support by impregnation into an impregnation solution containing noble metal ions by impregnation method, and the impregnation solution includes chloroplatinic acid 40 5 parts, 5 parts of rice furoic acid, 3 parts of dichlorophenyl imidazole dioxolane, the load on the solid carrier is 5% of the weight of the solid carrier;
[0037] Step S3: Dehydrogenation reaction of piperidine ring: (R,R)-8-benzyl-2,8-diazabicyclo[4,3,0]nonane obtained by optical resolution and platinum dehydrogenation catalyst At a reaction ...
Embodiment 3
[0040] The preparation process of racemic cis 8-benzyl-2,8-diazabicyclo[4,3,0]nonane comprises the following steps:
[0041] Step S1: preparing an attachment carrier: immersing the solid carrier into a roughening solution to prepare an attachment carrier, the roughening solution being sodium hydroxide solution or sodium bifluoride solution;
[0042] Step S2: Prepare the platinum dehydrogenation catalyst: use the impregnation method to load the noble metal platinum on the silica-alumina colloidal solid support by impregnating into the impregnating solution containing noble metal ions. The impregnating solution includes chloroplatinic acid 35 3 parts, 3 parts of rice furoic acid, 2 parts of dichlorophenyl imidazole dioxolane, the load on the solid carrier is 2% of the weight of the solid carrier;
[0043] Step S3: Dehydrogenation reaction of piperidine ring: (R,R)-8-benzyl-2,8-diazabicyclo[4,3,0]nonane obtained by optical resolution and platinum dehydrogenation catalyst At a re...
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