Synthetic Route of 63131-30-6, These common heterocyclic compound, 63131-30-6, name is Ethyl 3-(4-iodophenyl)-3-oxopropanoate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
The reaction was as follows: In a nitrogen atmosphere, palladium trifluoroacetate (0.33 mg, 2 mumol) and L3 (1.1 mg, 2.4 mumol) were mixed in a glove box, 1 mL of degassed acetone was added, and the mixture was stirred at room temperature for 1 hour, and the solvent was drained to obtain The in-situ generated metal complex was dissolved with 0.5 mL of pentafluoropropanol, added to a hydrogenation bottle, and 4i (20 mg, 0.1 mmol) was added, and the hydrogenated bottle was transferred to an autoclave. After the reaction vessel was closed, hydrogen was replaced three times, hydrogen gas was charged to 30 atm, and the reaction was carried out at 0 C. for 20 hours and then returned to room temperature. The hydrogen was vented and the reactor was opened. The crude reaction solution was filtered through a microporous membrane to remove metal ions. After diluting with isopropanol, the conversion rate and the product (R)-3-hydroxyl were directly determined by HPLC with a chiral AD-H column. Ethyl-3-(4-iodophenyl)propionate [(R)-5i] has an ee value of 97%.
Statistics shows that Ethyl 3-(4-iodophenyl)-3-oxopropanoate is playing an increasingly important role. we look forward to future research findings about 63131-30-6.
Reference:
Patent; Chinese Academy Of Sciences Shanghai Organic Chemistry Institute; Tang Wenjun; Jiang Wenhao; (37 pag.)CN107827929; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com