Synthetic method of zinc pyrrolidone carboxylate
A technology of zinc pyrrolidone carboxylate and pyrrolidone carboxylic acid is applied in the field of synthesis of zinc L-pyrrolidone carboxylate, can solve the problems of low yield, unsatisfactory PCA-Zn, and high cost, and achieves low reaction temperature, low cost, Not easy to racemization effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0027] Add 50g of L-glutamic acid into a 100mL flask, immerse in a preheated 140°C oil bath, and pass through N 2 Take water, flow out until there is no water, TLC detects that the raw material L-glutamic acid has reacted completely; cool the reaction product to 50-60°C, add 30mL of deionized water, slowly add 21.0g of zinc carbonate solid under stirring, and Incubate at high temperature for 2 hours, TLC detects no L-pyrrolidone carboxylic acid exists, stop the reaction and cool to room temperature, precipitate a large number of crystals, filter with suction, wash the filter cake with a small amount of cold water, and dry to obtain the first batch of products; the mother liquor is cooled to 0°C overnight , part of the crystals were precipitated again, and after suction filtration, washing and drying, they were combined with the first batch of products to obtain 45.0 g of PCA-Zn with a yield of 74.2%.
Embodiment 2
[0029] Add 50g of L-glutamic acid into a 100mL flask, immerse in a preheated 140°C oil bath, vacuum the water generated by the reaction, and TLC detects that the raw material L-glutamic acid has completely reacted; the reaction product is cooled to 50-60°C, add 40mL of deionized water, slowly add 28.0g of basic zinc carbonate solid (ZnCO 3 2Zn(OH) 2 ·H 2 (0), and kept at this temperature for 1.5h, TLC detects that no L-pyrrolidone carboxylic acid exists, stops the reaction and is cooled to room temperature, a large amount of crystals are separated out, suction filtered, and the filter cake is washed with a small amount of cold water and dried to obtain the first batch of products; The mother liquor was cooled to 0°C overnight, and some crystals were precipitated again. After suction filtration, washing and drying, it was combined with the first batch of products to obtain 46.6 g of PCA-Zn with a yield of 76.8%.
Embodiment 3
[0031] Add 50g of L-glutamic acid into a 100mL flask, immerse in a preheated 140°C oil bath, vacuum the water generated by the reaction, and TLC detects that the raw material L-glutamic acid has completely reacted; the reaction product is cooled to 10-20°C, add 50mL of deionized water, slowly add 22.0g of zinc carbonate solid under stirring, and keep warm at this temperature for 3.5h, TLC detects that there is no L-pyrrolidone carboxylic acid, stop the reaction and cool to room temperature, and a large amount of Crystal, suction filtration, the filter cake was washed with a small amount of cold water, and dried to obtain the first batch of products; the mother liquor was cooled to 0°C overnight, and part of the crystals were precipitated again, after suction filtration, washing and drying, combined with the first batch of products to obtain PCA -Zn 43.8q, yield 73.8%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More