Extracurricular laboratory: Synthetic route of Ethyl 3-Hydroxypropanoate

At the same time, in my other blogs, there are other synthetic methods of this type of compound,623-72-3, Ethyl 3-Hydroxypropanoate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 623-72-3, Ethyl 3-Hydroxypropanoate, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, SDS of cas: 623-72-3, blongs to alcohols-buliding-blocks compound. SDS of cas: 623-72-3

EXAMPLE 42 In 5 ml of tetrahydrofuran was dissolved 1.12 g of diethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine- 3,5-dicarboxylate and after adding to the solution 0.17 g of 50% oil dispersion of sodium hydride at room temperature, the resultant mixture was stirred for 30 minutes at room temperature. Then, the mixture was cooled to -30 C., and after adding dropwise thereto 0.74 g of 1,3-propansultone, the temperature of the system was raised till room temperature and the reaction mixture was stirred for 3 days at room temperature. The reaction solution was concentrated and the precipitate formed was washed with 30 ml of ether. This precipitate was dissolved in 2 ml of water and the solution obtained was subjected to a silica gel (30 g) column chromatography. After eluding the small amount of raw material using ethyl acetate as an elute, the product was then developed by using 1:1 ethyl acetatemethanol mixed solvent as an elute and the solvent of the effluent was distilled away under reduced pressure. To the residue obtained was added 2 ml of water and after cooling, the crystal formed was filtered to provide 0.35 g of sodium alpha-[2,6-dimethyl-3,5-bis(ethoxycarbonyl)-4-(3-nitrophenyl)-1,4-dihydropyridin-1-yl] propylsulfonate. Nuclear magnetic resonance (CDCl3): signal of 6.0 PPM of raw material (1H, S, proton at 1-position) vanished.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,623-72-3, Ethyl 3-Hydroxypropanoate, and friends who are interested can also refer to it.

Reference:
Patent; Yamanouchi Pharmaceutical Co., Ltd.; US4021434; (1977); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Some tips on 623-72-3

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 623-72-3, Ethyl 3-Hydroxypropanoate.

623-72-3, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 623-72-3, name is Ethyl 3-Hydroxypropanoate. This compound has unique chemical properties. The synthetic route is as follows.

Example 16 This example describes the preparation of various alkyl acrylate esters by dehydrating 3-HP esters using various catalysts. A catalyst was placed in a 3-neck flask that was equipped with a temperature probe (in contact with the catalyst). A distillation column and receiving flask were attached so that the vapors formed during the reaction could be collected, and the catalyst was heated to the desired temperature. A solution of a 3-hydroxypropionic acid ester in the corresponding alcohol was added drop-wise directly onto the catalyst using a syringe. The liquid that distilled over was collected and analyzed by gas chromatography. The results, and corresponding experimental conditions are shown in the following table. Ester Catalyst Temperature Concentration Solvent Yield of Yield of (C) of Ester in Acrylic Acrylic Solvent ester (GC) acid (GC) – (%) (%) (%) Ethyl NaH2P04-Silica 275-EtOH 49 26 Ethyl NaH2PO4-Silica 250 35 EtOH 53 Ethyl NaH2PO4-Silica 250 50 EtOH 14 21 Ethyl NaH2PO4-Silica 180 40 EtOH 30 – Ethyl Copper-H3PO4 220 20 EtOH 50 50 Methyl NaH2PO4-Silica 280-MeOH 78 Methyl CuS04-Silica 280-MeOH 37 9 Methyl Cs2CO3-Silica 220 45 MeOH 49 – Butyl NaH2PO4-Silica 280 50 BuOH 40 Similar dehydration reactions were performed using 3-HP as the starting material and a flask containing heated catalyst in place of the GC: (a) Aqueous 3-HP was dehydrated to acrylic acid over NaH2PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 90- 96%. (b) Aqueous 3-HP was dehydrated to acrylic acid over H3PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 85-90%. (c) Aqueous 3-HP was dehydrated to acrylic acid over CuS04-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 73%. (d) Aqueous 3-HP was dehydrated to acrylic acid over Zeolite H-ss powder and 85% H3PO4 as the catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 71%. (e) Aqueous 3-hydroxyisobutyric acid was dehydrated to methacrylic acid over NaH2PO4-Silica gel catalyst at 270C. Based on GC analysis, the yield of methacrylic acid was 79%.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 623-72-3, Ethyl 3-Hydroxypropanoate.

Reference:
Patent; CARGILL, INCORPORATED; WO2003/82795; (2003); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

A new synthetic route of 623-72-3

The chemical industry reduces the impact on the environment during synthesis 623-72-3, I believe this compound will play a more active role in future production and life.

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 623-72-3 as follows., 623-72-3

Example 16 This example describes the preparation of various alkyl acrylate esters by dehydrating 3-HP esters using various catalysts. A catalyst was placed in a 3-neck flask that was equipped with a temperature probe (in contact with the catalyst). A distillation column and receiving flask were attached so that the vapors formed during the reaction could be collected, and the catalyst was heated to the desired temperature. A solution of a 3-hydroxypropionic acid ester in the corresponding alcohol was added drop-wise directly onto the catalyst using a syringe. The liquid that distilled over was collected and analyzed by gas chromatography. The results, and corresponding experimental conditions are shown in the following table. Ester Catalyst Temperature Concentration Solvent Yield of Yield of (C) of Ester in Acrylic Acrylic Solvent ester (GC) acid (GC) – (%) (%) (%) Ethyl NaH2P04-Silica 275-EtOH 49 26 Ethyl NaH2PO4-Silica 250 35 EtOH 53 Ethyl NaH2PO4-Silica 250 50 EtOH 14 21 Ethyl NaH2PO4-Silica 180 40 EtOH 30 – Ethyl Copper-H3PO4 220 20 EtOH 50 50 Methyl NaH2PO4-Silica 280-MeOH 78 Methyl CuS04-Silica 280-MeOH 37 9 Methyl Cs2CO3-Silica 220 45 MeOH 49 – Butyl NaH2PO4-Silica 280 50 BuOH 40 Similar dehydration reactions were performed using 3-HP as the starting material and a flask containing heated catalyst in place of the GC: (a) Aqueous 3-HP was dehydrated to acrylic acid over NaH2PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 90- 96%. (b) Aqueous 3-HP was dehydrated to acrylic acid over H3PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 85-90%. (c) Aqueous 3-HP was dehydrated to acrylic acid over CuS04-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 73%. (d) Aqueous 3-HP was dehydrated to acrylic acid over Zeolite H-ss powder and 85% H3PO4 as the catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 71%. (e) Aqueous 3-hydroxyisobutyric acid was dehydrated to methacrylic acid over NaH2PO4-Silica gel catalyst at 270C. Based on GC analysis, the yield of methacrylic acid was 79%.

The chemical industry reduces the impact on the environment during synthesis 623-72-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; CARGILL, INCORPORATED; WO2003/82795; (2003); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts