Reaction equation
P([O-])([O-])([O-])=O.C([NH:9][CH:10]([C:15]([OH:17])=[O:16])[CH2:11][CH2:12][S:13][CH3:14])(=O)C>[Co](Cl)Cl>[NH2:9][C@H:10]([C:15]([OH:17])=[O:16])[CH2:11][CH2:12][S:13][CH3:14]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 30 °C
Procedure
While maintaining the above column at 30° C., a 20 mM phosphate buffer containing 0.5% N-acetyl-DL-methionine and 1 mM cobalt chloride was flowed through the column at a flow rate of 30 ml per hour. 3 l of the effluent was collected and passed through IR 120 cation exchange resin, after which it was concentrated under reduced pressure until it was dry and solid. The obtained residue, after being washed twice with 10 ml of cool absolute alcohol, was dissolved in about 100 ml of hot water, and the crystal which separated during cooling was collected by filtration. Furthermore, alcohol was added drop-by-drop to the filtrate, and this mixture was kept standing overnight. The crystal which separated was collected and dried to obtain 9.6 g of L-methionine. The melting point was 280° to 281° C., [α]D25 -8.2°(c=1%). This product showed entirely the same behaviors as those of a standard sample of L-methionine in high performance liquid chromatography and thin layer chromatography. In addition, this product, when melted together with a standard sample, exhibited no drop of melting point.
Workup
- custom3 l of the effluent was collected
- concentrationafter which it was concentrated under reduced pressure until it
- customwas dry
- washThe obtained residue, after being washed twice with 10 ml of cool absolute alcohol
- dissolutionwas dissolved in about 100 ml of hot water
- customthe crystal which separated
- temperatureduring cooling
- filtrationwas collected by filtration
- additionFurthermore, alcohol was added drop-by-drop to the filtrate
- customThe crystal which separated
- customwas collected
- customdried
Sources & evidence
- ORD record
- ord-1467289178d64ccc812da26bb1b34d3a
- Source dataset
- uspto-grants-1991_01
- Patent number
- US04981799
Linked notes
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