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ChemicalBook CAS DataBase List N-Methylmethanamine 2,4-dichlorophenoxyacetate

N-Methylmethanamine 2,4-dichlorophenoxyacetate synthesis

8synthesis methods
-

Yield:2008-39-1 100%

Reaction Conditions:

Stage #1:2,4-Dichlorophenoxyacetic acid with ethylenediaminetetraacetic acid in tert-butyl methyl ether
Stage #2:dimethyl amine in tert-butyl methyl ether; pH=8 at 56;Product distribution / selectivity;

Steps:

6
Example 6; Process[0046] MTBE was charged into a reactor equipped with the overhead reflux condenser and a stirrer. The phenoxyacid, REAX83 and EDTA were added. The mixture was stirred for 15-20 minutes. Anhydrous DMA was added till solution reaches and remained at pH of above 8. During introduction of DMA, the reaction temperature rose to the boiling point of the MTBE (56°C). Product precipitation occurred during introduction of DMA. The resulting product slurry was cooled by water to 25°C and the precipitate collected as a wet cake in a centrifuge. The wet cake from centrifuge was dried in a drier while the mother liquor was recycled to the reactor for next batch. Fresh MTBE was added to the reactor to compensate for MTBE losses.Conclusion[0047] Table 1 below provides comparison for the ether and acetone processes. Table 1CE-A Example 6 (Acetone Process) (Ether Process)2,4-D (tech.) charge (kg) 4,000 4,000(bags) 5 5Reaction mass (kg) 14022 12829S.G. of solvent, g/mL 0.791 0.739Mass of dray final product (Yield) (Kg) 4341 4875Isolated yield (%) 92.5 100Active as 2,4-D (%) 82.4 79.8Formulation in situ Not Possible Yes

References:

NUFARM AUSTRALIA LIMITED;KRAVETS, Eduard WO2011/143690, 2011, A1 Location in patent:Page/Page column 10-11

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