Propanethiosulfonic acid S-propyl ester synthesis
- Product Name:Propanethiosulfonic acid S-propyl ester
- CAS Number:1113-13-9
- Molecular formula:C6H14O2S2
- Molecular Weight:182.3
107-03-9
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Yield:1113-13-9 87.7%
Reaction Conditions:
with dihydrogen peroxide;potassium bromide in water;acetone at 40; for 4 h;Reagent/catalyst;Temperature;
Steps:
1; 4 Example 1: Synthesis of 1-(propane-1-sulfonyl)sulfanyl propane
Add 300 g of acetone, 20 g of potassium bromide, 100 g of purified water and 76 g of n-propyl mercaptan to a 1 L three-necked flask at 25°C. The temperature of the system was raised to 40° C. and 340 g of hydrogen peroxide (30% content) was added dropwise to the above system. After the addition was completed, the system was kept and reacted for 4 hours until the GC showed that the purity of the product was more than 95%. The temperature of the reaction system was lowered to 20°C, and 300 g of methyl tert-butyl ether was added to the system for liquid separation. The upper organic phase was washed successively with purified water, 5% sodium sulfite and saturated brine; the organic phase was concentrated under reduced pressure (vacuum -0.09MPa, water bath at 40°C) until no low-boiling substances escaped, and 79.8g of concentrated liquid (which is the target compound) 1-(propane-1-sulfonyl)sulfanyl propane. The gas phase purity is 99.2%, and the yield is 87.7%.
References:
CN113620764,2021,A Location in patent:Paragraph 0030-0033; 0042-0044
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