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With hydrogen;palladium 10% on activated carbon; In methanol; water; under 3000.3 Torr;
EXAMPLE IX1-methyl-azetidine-3-carboxylic acid200 mg azetidine-3-carboxylic acid are dissolved in 10 ml of methanol, combined with 165 mul of a 37percent solution of formaldehyde in water as well as 20 mg 10percent palladium on charcoal and hydrogenated at 4 bar until the hydrogen uptake has ended.Then the catalyst is eliminated by suction filtering, the solvent is eliminated in vacuo, the residue is taken up in methanol and toluene and the solvents are again eliminated in vacuo.Yield: 214 mg (94percent of theory)Mass spectrum (ESI+): m/z=116 [M+H]+
With 10% palladium hydroxide on charcoal; hydrogen; In methanol; water; under 22502.3 Torr; for 6h;
78 g of the intermediate product (D) prepared in Example 3 was added to a mixture of 500 mL of methanol and 100 mL of water, 7 g of palladium hydroxide on carbon (10%) was added, and hydrogen gas was introduced into it to make the pressure of the reaction vessel reach 3 MPa After 6 hours of reaction, the reaction was complete, the catalyst was removed by filtration, 500 mL of water was added, the methanol was distilled off, the diphenylmethane was extracted twice with ethyl acetate, the water layer was concentrated to dryness, and the obtained solid was added to 300 mL of water again, and the pH was adjusted with potassium carbonate solid. 6.7 There is turbidity. Extract with ethyl acetate, dry the organic layer, and concentrate to dryness to obtain 25 g of azetidine-3-carboxylic acid as a solid product, with a yield of 85%.
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