Synthesis
1. 100 g (0.878 mol) of glutaric anhydride was dissolved in 50 mL of anhydrous methanol and heated to reflux for 1 h. 2. Upon completion of the reaction, unreacted methanol was removed by distillation under reduced pressure. 3. The reaction mixture was cooled to room temperature, and 200 mL of acetochloride was slowly added. 4. The reaction mixture was heated for 6 h., wherein after 2 h of heating the remaining dichloro sulfoxide.5. Finally, the fractions were dried at 96 °C to 98 °C/10 mmHg to give 124.2 g of methyl 4-chlorocarbonylbutyrate as a light yellow liquid in 86.4% yield.
References
[1] Patent: CN103864658, 2016, B. Location in patent: Paragraph 0056; 0057
[2] Tetrahedron Letters, 1984, vol. 25, # 39, p. 4371 - 4374
[3] Journal of Enzyme Inhibition and Medicinal Chemistry, 2016, vol. 31, # 6, p. 915 - 923
