Triphenylphosphine-3,3',3''-trisulfonic acid trisodium salt synthesis
- Product Name:Triphenylphosphine-3,3',3''-trisulfonic acid trisodium salt
- CAS Number:63995-70-0
- Molecular formula:C18H16NaO9PS3
- Molecular Weight:526.46
603-35-0
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63995-70-0
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Yield:63995-70-0 98.6%
Reaction Conditions:
Stage #1: triphenylphosphinewith chlorosulfonic acid;sulfuric acid at 0 - 25;
Stage #2: with sodium hydroxide in water at 60;Temperature;Reagent/catalyst;
Steps:
1-3; 1-3 Example 1
To prepare trisulfonated triphenylphosphine (TPPTS), follow the steps below:Add 160g sulfuric acid into the reaction flask, stir and cool,Start adding 40g TPP (0.15 mol) at T=0°C, and maintain the temperature at 05°C. After the reaction solution is stirred and dissolved,Start adding 70g of chlorosulfonic acid (0.6mol) dropwise, and the temperature does not exceed 10°C, and the addition is complete.Continue to stir the reaction for 19-20 hrs, keep the reaction temperature at about 25°C, and basically complete the reaction as detected by HPLC.The reaction solution was slowly added to 200 g of water, and the temperature of the dropwise addition did not exceed 10°C.After the addition, 200ml of tributyl phosphate × 2 was added for extraction twice, and the organic layers were combined.The organic layer was adjusted to pH=7-8 with a 5% sodium hydroxide aqueous solution, and the liquid was separated. The aqueous layer was concentrated under reduced pressure at 60°C until a solid precipitated.1000ml of methanol was added and stirred to precipitate solids, filtered again, and the filtrate was concentrated to dryness under reduced pressure at 60°C to obtain about 90 g of crude TPPTS.Add 90 g of water to dissolve the solution, add 1000 ml of ethanol, stir and crystallize for 2 hours, and filter. The product is air-dried at 40°C. 85.5 g of the product was obtained, with a yield of 98.6% and a purity of 98.956% as determined by HPLC.
References:
CN112724170,2021,A Location in patent:Paragraph 0009; 0024-0044; 0050
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63995-70-0
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63995-70-0
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