Methylamine hydrochloride synthesis

9synthesis methods

Product Name:Methylamine hydrochloride
CAS Number:593-51-1
Molecular formula:CH5N.ClH
Molecular Weight:67.52

Methylamine hydrochloride is prepared by heating a mixture of aqueous formaldehyde and ammonium chloride; the residual water and the formic acid produced in the reaction are removed via vacuum distillation. This leaves behind solid methylamine hydrochloride. The solid is then purified by organic extractions and additional vacuum distillations. Methylamine gas for the reaction with P2P is generated in situ by heating the hydrochloride salt with sodium hydroxide. Alternatively, methylamine can be liberated from the hydrochloride with base and collected in a cold finger or flask immersed in a dry ice bath.

56-40-6 Synthesis

56-40-6
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$5.00/25g

593-51-1
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$21.00/100g

Yield:593-51-1 86%

Reaction Conditions:

Stage #1: glycinewith (R)-Carvone in propan-1-ol at 20 - 190; under 11251.1 Torr; for 0.216667 h;Sealed tube;Microwave irradiation;
Stage #2: with hydrogenchloride in propan-1-ol;water at 190; for 0.0833333 h;Microwave irradiation;

Steps:

General “One-Pot” Procedure for the Decarboxylation of Amino Acids

General procedure: General “One-Pot” Procedure for the Decarboxylation of Amino Acids [0045] A magnetic stir bar, 3 mL of n-PrOH, 10 mmol of R-Carvone, and 5 mmol of amino acid were charged to a pressure vessel. The vessel was heated from room temperature to 190° C. over 5 min with stirring. If necessary the reaction vessel was maintained at 190° C. for additional time until the slurry became clear. The vessel was allowed to cool to below the solvent boiling point, carefully vented to release evolved CO₂, and 10 mL of 2M HCl was added. The vessel was heated to 190° C. over 5 min with stirring and allowed to cool. The aqueous reaction mixture was washed three times with 25 mL of ether and water solvent distilled off from the hydrochloride salt. The hydrochloride salt was transferred to a vacuum oven and dried overnight at 150° C. and 10 Torr. The hydrochloride salt was then weighed and analyzed via IR and NMR.; methylamine hydrochloride, δ_H2.44 s; δ_C24.5

References:

US2014/275569,2014,A1 Location in patent:Page/Page column 0045; 0046; 0066; 0067

74-89-5 Synthesis