2-(3-CHLORO-5-TRIFLUOROMETHYL-PYRIDINYL)-MALONIC ACID DIMETHYL ESTER synthesis

Yield:477859-76-0 94.7%

Reaction Conditions:

Stage #1: 2,3-dichloro-5-trifluoromethylpyridinewith sodium carbonate in N,N-dimethyl-formamide at 55; for 1.9 h;
Stage #2: malonic acid dimethyl ester in N,N-dimethyl-formamide at 60; for 12 h;Temperature;

Steps:

2.1; 2.2; 2.3 Example 2 A method for synthesizing 2-(3-chloro-5-trifluoromethylpyridine)-malonate dimethyl ester, comprising the following steps:

Step 1, mixing 70 g of dimethylformamide and 70 g of 2,3-dichloro-5-trifluoromethylpyridine to obtain a mixture;Step 2, the mixture was added to 100 g of anhydrous sodium carbonate, stirred at 95 rpm for 24 minutes, heated to 55 ° C and incubated for 1.5 hours, and 44 g of dimethyl malonate was added dropwise over 30 minutes. The reaction was continued for 12 hours at 60 ° C to obtain a pale yellow paste;Step 3, the light yellow paste was cooled to 25 ° C, 800 g of water at 0 ° C was added, stirred at 95 rpm for 1.2 hours, and suction filtered at -0.087 MPa for 13 minutes, followed by drying at 40 ° C. 11 hours, the content was 98.2%2-(3-chloro-5-trifluoromethylpyridine)-dimethyl malonate,The yield was 94.7%

References:

CN108752268,2018,A Location in patent:Paragraph 0027-0050