Pyridoxal phosphate synthesis
- Product Name:Pyridoxal phosphate
- CAS Number:54-47-7
- Molecular formula:C8H10NO6P
- Molecular Weight:247.14
65-22-5
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54-47-7
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Yield:54-47-7 76%
Reaction Conditions:
Stage #1: pyridoxal hydrochloridewith N,N-dimethylethylenediamine in 5,5-dimethyl-1,3-cyclohexadiene at 90; for 8 h;
Stage #2: with polyphosphoric acid at 70; for 12 h;Solvent;
Steps:
2.2; 2.3
Step 2. Preparation of pyridoxal condensateThe 88 g of pyridoxal hydrochloride and 55 g of N,N-dimethylethylenediamine were added to 880 mL of xylene and stirred to warm upThe reaction was carried out at 90° C. and refluxed for 8 h. After the reaction was complete, the toluene was concentrated in vacuo to give a concentrate 2 which was added to the concentrate 2 .Distilling 200 mL of methylene chloride, heating up to dissolution, then cooling the crystals to obtain 85 g of pyrofalaldehyde condensate;Step 3. Preparation of pyridoxal phosphate85g of pyridoxal condensate and 120g of polyphosphoric acid were added to the reaction flask, and the reaction mixture was stirred and warmed to 70°C for 12h to react.Completely, then add 60mL of water and stir evenly. Pass 550mL of 732 resin. The resolution flow rate is 0.2BV/h.In 83% of the analytical solution, concentrated under reduced pressure to give a concentrate 3, to the concentrate 3 was added 340 mL of n-propanol to dissolve, slowly coolingWhite crystals were obtained and dried to give 76 g of the product pyridoxal phosphate. The total mass yield was 76%.
References:
CN107652323,2018,A Location in patent:Paragraph 0023; 0024
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