Diethyl (tosyloxy)methylphosphonate synthesis
- Product Name:Diethyl (tosyloxy)methylphosphonate
- CAS Number:31618-90-3
- Molecular formula:C12H19O6PS
- Molecular Weight:322.31
3084-40-0
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$10.00/10g
104-15-4
734 suppliers
$133.00/500g
31618-90-3
429 suppliers
$5.00/5g
Yield:31618-90-3 337 g
Reaction Conditions:
in toluene at 4 - 5; for 2.16667 h;Alkaline conditions;Temperature;
Steps:
3.3-3.5
(3) Reduce the temperature of the material in the bottle to about 2°C; add 250.0ml of toluene, add 210.0g of p-toluenesulfonyl chloride under stirring, and stir for 10 minutes; add 170.0ml of 30% alkali solution dropwise, and control the inside of the reaction bottle during the dropping process The material temperature is about 5, and the dripping time is 1.0 hour;(4) Incubate the materials in (3) at 4°C for 1 hour, take samples and check HPLC, until the content of p-toluenesulfonyl chloride in the reaction solution is less than 0.1% as the end of the reaction; let stand for 30 minutes, separate the liquid, and place the upper organic phase for a while Use, the lower aqueous phase is extracted with 350.0ml of toluene;(5) Combine the two organic phases, add 60.0 ml of 5% sodium chloride aqueous solution to wash, and concentrate the organic layer under reduced pressure. Obtained 337.0g of liquid product (purity 99%), and 585.0ml of toluene was recovered, which can be directly used in the next batch of reaction.
References:
CN113121596,2021,A Location in patent:Paragraph 0092-0094; 0097-0106; 0110-0115; 0119-0125
50-00-0
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762-04-9
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98-59-9
591 suppliers
$9.00/5g
31618-90-3
429 suppliers
$5.00/5g
3084-40-0
249 suppliers
$10.00/10g
31618-90-3
429 suppliers
$5.00/5g
