Synthetic Route of 10061-02-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 10061-02-6 as follows.
EXAMPLE 1; 382 g (406 ml) of DMF were initially charged in a Schmizzo and 137 g (141 ml) of 1.0 eq. NaOMe (30% solution in methanol) were added. This mixture was then heated to 60 C. (+/-3 C.) and 131 g (0.753 mol) of dimethyl isopropylmalonate were metered in within one hour. Subsequently, a methanol/DMF mixture (201 g) was distilled off under pressure (300 mbar to 60 mbar) and a temperature of 60 C.Thereafter, at 80 C. (+/-3 C.), 86 g (79 ml, 0.779 mol, 1.03 eq.) of 1,3-dichloropropene were metered in within one hour and the reaction mixture was then heated at 80 C. (+/-3 C.) for two hours. The reaction mixture was heated to 140 C. and a 25% solution of LiCl (0.6 eq.) in methanol (19 g of LiCl in 58 g of methanol) was metered in within two hours, and the reaction mixture was heated at 140-142 C. for a further 6 hours, in the course of which a portion of the methanol was distilled off and approx. 1.5 mol of gas (mainly CH3Cl and CO2) formed. The maximum amount of gas in the first half hour was approx. 6 liters. On completion of reaction, the solvent (DMF) and the excess methanol were distilled off substantially fully under reduced pressure. The remainder was admixed with 200 g of water, 89 g of 34% HCl and 200 g of MTBE, and the phases were separated. The organic phase was washed lx with 50 g of water and the solvent was removed under reduced pressure. Approx. 140 g of product were obtained, of which approx. 125 g were ester and 13 g the corresponding acid.
According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; DSM Fine Chemicals Austria NFG GMBH & Co KG; US2008/207943; (2008); A1;,
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