4-(Chloromethyl)-phenylacetic acid methyl ester synthesis
- Product Name:4-(Chloromethyl)-phenylacetic acid methyl ester
- CAS Number:95360-33-1
- Molecular formula:C10H11ClO2
- Molecular Weight:198.65
Yield:95360-33-1 191 g
Reaction Conditions:
at 20; for 1 h;Cooling with ice;
Steps:
1.1; 2.1; 3.1 (1) Synthesis of methyl 2-chloromethylphenylacetate
476 g of thionyl chloride (molecular weight 119.0, 4.0 mol) was added to the four-necked flask, and 148 g of 3-isochromone (molecular weight: 148.2, 1.0 mol) was heated and refluxed for 4 hours, and the content of 3-isochromone was detected by GC. 0.3% is qualified; after passing, the negative pressure distillation of thionyl chloride is dried to obtain 201 g of 2-chloromethylphenylacetyl chloride in brown oil; the other four vials are added with 256 g of methanol (molecular weight 32,8.0 mol), ice. The water is cooled to below 20 ° C, 2-chloromethyl phenyl acetyl chloride is added dropwise, and acid gas is emitted and the heat is released.Strong, the temperature is 1 hour after the completion of the test to detect the complete reaction of the raw materials, and the methanol is removed by vacuum.Obtained 191.0 g of methyl 2-chloromethylphenylacetate with a qualitative content of 98.1%.Yield 95.5%(molecular weight 196.6, 0.947 mol);
References:
CN109748792,2019,A Location in patent:Paragraph 0027; 0028; 0029; 0032; 0033; 0034; 0037-0039
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