Method for chemical synthesis of vitamin K2
A chemical synthesis and vitamin technology, applied in organic chemistry, quinone oxide preparation, etc., can solve the problems of high equipment requirements, difficult separation, large amount of eluent and adsorbent, etc., and achieve equipment and energy consumption reduction, separation The treatment is simple and beneficial to the effect of environmental protection
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Embodiment 1
[0029] A chemically synthesized vitamin K 2 The method, its specific method steps are as follows:
[0030] (1) Catalytic hydrogenation reduction reaction
[0031] With 2-methyl-1,4-naphthoquinone as raw material, Pd / C with a mass concentration of 5% as a catalyst, and isopropyl ether as a solvent, according to the molar amount of 2-methyl-1,4-naphthoquinone (mol): the volume (ml) of isopropyl ether: the ratio of the mass (g) of 5% Pd / C is the ratio of 1: 5000: 20, in the dry reflux reactor with stirring device, add 2 -Methyl-1,4-naphthoquinone and isopropyl ether and stir and mix evenly, then pass through nitrogen protection, and heat until the reaction liquid starts to reflux, and under the condition of maintaining reflux, switch nitrogen to hydrogen to the entire reactor Until the inside is filled with hydrogen, then under stirring conditions, add a Pd / C catalyst with a mass concentration of 5%, and continue to pass hydrogen to carry out the catalytic hydrogenation reducti...
Embodiment 2
[0040] A chemically synthesized vitamin K 2 The method, with embodiment 1, wherein:
[0041] In the (1) step, the molar weight (mol) of 2-methyl-1,4-naphthoquinone: the volume (ml) of isopropyl ether: the ratio of the mass (g) of the Pd / C of 5% is 1: 4000:15, the collected filtrate was distilled at a constant temperature of 70°C to recover the solvent isopropyl ether, and the distilled product was placed in a vacuum desiccator, and vacuum-dried at 95°C for 0.75 hours.
[0042] (in the 2nd step, the molar weight (mol) of geraniol: the molar weight (mol) of the 2-methyl-1,4-naphthalenediol that (1) step reaction makes: the volume of solvent isopropyl ether (ml): water-resistant Lewis acid catalyst (ie Sm(OTf) 3 ) in a molar (mol) ratio of 1:1:4000:0.05, the Fridel-Crafts alkylation reaction was carried out at a constant temperature of 40° C. for 6 hours. The ratio of reaction liquid: volume (ml) of distilled water was 1:0.5, and the ratio of organic layer: volume (ml) of dist...
Embodiment 3
[0046] A chemically synthesized vitamin K 2 The method, with embodiment 1, wherein:
[0047]In the (1) step, the molar weight (mol) of 2-methyl-1,4-naphthoquinone: the volume (ml) of isopropyl ether: the ratio of the mass (g) of the Pd / C of 5% is 1: 6000:25, the collected filtrate was distilled at a constant temperature of 71°C to recover the solvent isopropyl ether, and the distilled product was placed in a vacuum desiccator, and vacuum-dried at 100°C for 0.5 hours.
[0048] (in the 2nd step, the molar weight (mol) of geraniol: the molar weight (mol) of the 2-methyl-1,4-naphthalenediol that (1) step reaction makes: the volume of solvent isopropyl ether (ml): water-resistant Lewis acid catalyst (ie Sm(OTf) 3 ) in a molar (mol) ratio of 1:2:6000:0.2, the Fridel-Crafts alkylation reaction was carried out at a constant temperature of 40° C. for 3 hours. The ratio of reaction solution: volume (ml) of distilled water was 1:1, the ratio of organic layer: volume (ml) of distilled ...
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