Electric Literature of 108078-14-4, 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 108078-14-4 as follows.
A 100-mL RB flask was charged with 2-iodo-3-methylbenzoic acid (1. LG, 4.2 mmol), a stirbar, Et20 (15 mL) and DCM (35 mL) and was cooled to-78 oC under an argon atmosphere. trifluoromethanesulfonic acid (250 uL) was added over 30 sec and isobutylene was bubbled into the solution (until the solution became cloudy) using a 8″/20 gauge steel needle. The reaction was stirred for 6 h between-78 AND-20 oC. Solid NAHCO3 (250 mg) was added and the solution was allowed to warm to rt with stirring. After 20 min, the solution was poured into an extraction funnel containing DCM (50 mL) and NA2C03 (2M, 20 mL). The layers were separated and the organic layer was washed with NA2C03 (2M, 2 x 10 mL), water (20 mL), brine (30 mL) and dried over sodium sulfate. Removal of the solvent in vacuo yielded the title compound (1.05 g, 78%) which was used without further purification. 1H-NMR (CDC13) : delta 7.25 (m, 3H), 2.50 (s, 3H), 1.62 (m, 9H).
According to the analysis of related databases, 108078-14-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; 3-DIMENSIONAL PHARMACEUTICALS, INC.; WO2003/99805; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com