Yield:4316-73-8 97.2%

Reaction Conditions:

with sodium hydroxide;Cu/Ni Raney catalyst in water at 160; under 7500.75 Torr; for 4 h;

Steps:

1

10 g (calculated on the basis of the dry substance) of a Cu/Ni-based Raney catalyst (Degussa AG, BOO 111) was placed first as a suspension in water in a 600 ml autoclave with stirrer, pressure control valve and jacket heating and 75 g N-methyl-ethanolamine as well as 204 g of a 20% by weight sodium hydroxide solution were added. The autoclave was closed and the contents were heated to a temperature of 160° C. with the aid of the jacket heating. An increasing pressure of hydrogen was generated in this process which was kept at 10 bar (absolute) by the controlled opening of the pressure control valve. The release of gas was completely finished after 4 hours and the reactor was cooled to 90° C. After the stirrer was switched off, the catalyst sedimented within one hour and a portion of the supernatant clear solution of Na sarcosinate was moved from the autoclave through a plunge pipe. The catalyst remained in the reactor and could be used again in further batches.For each further cycle the suspension of catalyst remaining in the reactor was admixed with the said amounts of N-methylethanolamine and sodium hydroxide solution and the reaction was started by heating.With the exception of the initial batch, 270 g of a colourless solution of Na sarcosinate containing 40.0% by weight (corresponds to a yield of 97.2% of theory) was obtained per cycle.

References:

US2009/163739,2009,A1 Location in patent:Page/Page column 2