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ChemicalBook CAS DataBase List Methyl 3-mercaptopropionate
2935-90-2

Methyl 3-mercaptopropionate synthesis

6synthesis methods
The traditional synthetic method of the Methyl 3-mercaptopropionate comprises the steps of adding 2% -5% of concentrated sulfuric acid as a catalyst in an inert atmosphere, refluxing (65-70 ℃) for a reaction for 15 hours, evaporating reaction liquid to remove methanol after the reaction is finished, and then deacidifying; during the deacidification process, a large amount of deionized water is added for water washing, and when the pH of the water washing solution is close to neutrality, the Methyl 3-mercaptopropionate product is obtained by reduced pressure distillation. Another method for preparing Methyl 3-mercaptopropionate is by using a reactive distillation technology. Mix the reactant 3-mercaptopropionic acid and methanol, then perform pre-reaction through a fixed bed reactor filled with a catalyst to obtain a crude product of the methyl 3-mercaptopropionate. The crude product is pumped to the middle part of the reaction rectifying tower by a feeding pump and is input; fresh methanol and a water-carrying agent are input from the lower part of the reaction rectifying tower, a catalyst is arranged at the lower part of the reaction rectifying tower, and unreacted 3-mercaptopropionic acid in the crude product continuously reacts with methanol in a catalyst bed layer of the reaction rectifying tower; after the reaction is finished, excess methanol, water carrying agent and water are extracted from the upper part of the reaction rectifying tower, and the product Methyl 3-mercaptopropionate is extracted from the bottom of the tower.
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Yield:2935-90-2 94.6%

Reaction Conditions:

with 1-methyl-3-(3-sulfopropyl)imidazol-3-ium hydrogen sulfate at 50; for 0.00277778 h;Catalytic behavior;Flow reactor;Large scale;Temperature;

Steps:

1 Example 1

Weigh 1810 g of methanol, 2000 g of 3-mercaptopropionic acid, and 100 g of catalyst, mix 3-mercaptopropionic acid and catalyst evenly, and pump methanol, 3-mercaptopropionic acid, and catalyst solution into the microchannel reactor respectively, at 50° C. The reaction was carried out, the feeding speed of the pump was adjusted, the molar ratio of 3-mercaptopropionic acid and methanol was controlled to be 1:3, and the residence time was 10 seconds.After receiving the reaction material, the liquid was left to stand for stratification, and the upper reaction liquid was distilled and separated to obtain 2139.9 g of methyl 3-mercaptopropionate, and the calculated yield was 94.6%.The mass of the lower ionic liquid after dehydration is 210 g, and the content of mercaptopropionic acid is 51.4% in quantitative analysis.

References:

CN114773241,2022,A Location in patent:Paragraph 0018-0021

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