Method for synthesis of PMPA by combining biological technique and chemical technique
A chemical method, biological method, applied in the directions of biochemical equipment and methods, microorganism-based methods, chemical instruments and methods, etc., can solve the problems of unreachable and high production costs, and achieve simple post-processing and mild reaction conditions. , significant economic and social benefits
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Embodiment 1
[0029] (1) Preparation of R-chloropropanol (I)
[0030] Add 10g Angel dry yeast to 150ml pH=5.91 buffer solution, place the reaction flask in a shaker at T=35℃, activate for 0.5 hours, add 0.9g chloroacetone, and sample with a centrifuge tube every 0.5h , 3mL each time; after sampling, centrifuge with a centrifuge, the speed of the centrifuge is: r=4000rpm, time t=20min; after centrifugation, take the supernatant liquid, evaporate it with a rotary evaporator, and add methanol to dissolve and let it stand still ; Do temperament analysis. When the reaction is complete, centrifuge and concentrate, add 50ml methanol to dissolve, filter and concentrate to obtain 0.65g of chloropropanol (I).
[0031] (2) Preparation of (R)-2-[bis-(isopropyl)-phosphonomethoxy]-propyl chloride (II)
[0032] Put 9.4g (100mmol) of compound (I) in a 200ML three-necked flask, add 100ML of anhydrous THF, under ice bath, add 2.88g (120mmol), 60% NaH in batches, stir for 0.5 hour, then slowly add 38.2 dropwise ...
Embodiment 2
[0038] (1) Preparation of R-chloropropanol (I)
[0039] Add 10g Angel dry yeast to 150ml pH=6.98 buffer solution, place the reaction flask in a shaker at T=35℃, activate for 0.5 hours, add 0.9g chloroacetone, and sample with a centrifuge tube every 0.5h , 3mL each time; after sampling, centrifuge with a centrifuge, the speed of the centrifuge is: r=4000rpm, time t=20min; after centrifugation, take the supernatant liquid, evaporate it with a rotary evaporator, and add methanol to dissolve and let it stand still ; Do temperament analysis. When the reaction is complete, centrifuge and concentrate, add 50ml methanol to dissolve, filter and concentrate to obtain 0.80g of chloropropanol (I).
[0040] (2) Preparation of (R)-2-[bis-(isopropyl)-phosphonomethoxy]-propyl chloride (II)
[0041] Put 9.4g (100mmol) of compound (I) in a 200ML three-necked flask, add 100ML of anhydrous THF, add 6.0g (150mmol) NaOH in batches under ice bath, stir for 0.5 hour, and then slowly drop 38.2g (120mmol)...
Embodiment 3
[0047] (1) Preparation of R-chloropropanol (I)
[0048] Add 10g Angel dry yeast to 150ml pH=8.04 buffer solution, place the reaction flask in a shaker at T=35℃, activate for 0.5 hours, add 0.9g chloroacetone, and sample with a centrifuge tube every 0.5h , 3mL each time; after sampling, centrifuge with a centrifuge, the speed of the centrifuge is: r=4000rpm, time t=20min; after centrifugation, take the supernatant liquid, evaporate it with a rotary evaporator, and add methanol to dissolve and let it stand still ; Do temperament analysis. After the reaction is complete, centrifugal concentration, add 50ml methanol to dissolve, filter and concentrate to obtain 0.89g of chloropropanol (I).
[0049] (2) Preparation of (R)-2-[bis-(isopropyl)-phosphonomethoxy]-propyl chloride (II)
[0050] Put 9.4g (100mmol) of compound (I) in a 200ML three-necked flask, add 100ML of anhydrous THF, add 6.0g (150mmol) NaOH in batches under ice bath, stir for 0.5 hour, and then slowly drop 38.2g (120mmol)...
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