3-Carbamoymethyl-5-methylhexanoic acid synthesis
- Product Name:3-Carbamoymethyl-5-methylhexanoic acid
- CAS Number:181289-15-6
- Molecular formula:C9H17NO3
- Molecular Weight:187.24
185815-59-2
181289-15-6
The general procedure for the synthesis of 3-(aminocarbonylmethyl)-5-methylhexanoic acid using 4-isobutyldihydro-2H-pyran-2,6(3H)-dione as a starting material was as follows: first, 70 g of the dried product of 3-isobutylglutaric acid was reacted with 70 g of acetic anhydride at 120 °C for 2 h to produce 3-isobutylglutaric anhydride. Subsequently, 75g of 3-isobutylglutaric anhydride solution was slowly added dropwise to 180g of ammonia, and the temperature was controlled at 10°C during the reaction. After the dropwise addition, the reaction was continued for 2 hours. After the completion of the reaction, the pH of the solution was adjusted to 2~3 with hydrochloric acid, and a white powdery solid was obtained by filtration, i.e., the target product 3-isobutylglutaric acid monoamide. Liquid phase detection of the product showed a purity of 99.8%, a yield of 95% and an overall yield of 77.5%. Figure 4 illustrates the liquid phase assay results of 3-isobutylglutaric acid monoamide.
185815-59-2
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181289-15-6
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Yield:181289-15-6 100%
Reaction Conditions:
with ammonia in water at -10 - 40; for 1.5 h;
Steps:
1-9 Example 2:
At -10 to 12°C, 50 g of 3-isobutylglutaric anhydride is added dropwise to 36 g of concentrated ammonia water with a mass fraction of 25% to 28%, the temperature is raised to 30 to 40°C, and the temperature is kept for 1.5 hours. Add 50g of recovered wastewater, add 35% sulfuric acid solution dropwise at 20-40°C, adjust pH=2.0-3.0, stir for 10min, retest pH=2.0-3.0. After adding 120 ml of toluene mother liquor to extract the materials, the water layer is then extracted with 90 ml of toluene mother liquor, and the layers are combined. About 80ml of toluene was distilled off under reduced pressure. The temperature is lowered to 5-15°C, the temperature is kept for 1.5-2h, suction filtration, the filter cake is dried, the net weight is 55.0g, the yield is 100.0%, and the purity is 99.6%.
References:
CN105085302,2020,B Location in patent:Paragraph 0032-0049
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