Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 696-41-3, name is 3-Iodobenzaldehyde, A new synthetic method of this compound is introduced below., Quality Control of 3-Iodobenzaldehyde
General procedure: In the glove box, zinc powder (206.0 mg, 3.15 mmol) was added into a Schlenk tube. Anhydrous DMF (10.5 mL) was added and the mixture was stirred at room temperature. Chlorotrimethylsilane (66.5 muL, 0.52 mmol) was then added into the mixture to activate zinc powder. Five minutes later, PhSO2CF2Br (2) (2.1 mmol) was added into the suspension. The reaction proceeded smoothly in 15 min to give (phenylsulfonyl)difluoromethylzinc reagent (?XZnCF2SO2Ph?, 3). The mixture was kept at room temperature to precipitate the remaining zinc powder, and the solution was directly used for next step. In the glove box, 2-naphthaldehyde (156.2 mg, 1.0 mmol) was added into another Schlenk tube. Anhydrous DMF (5 mL) was added and the mixture was stirred at room temperature. The DMF solution of ?XZnCF2SO2Ph? (3) (10 mL, corresponding to the reaction of ca. 2.0 mmol of PhSO2CF2Br and ca. 3.0 mmol of zinc powder) was added to the solution of 2-naphthaldehyde dropwise. The mixture was stirred at room temperature for 5 h, and aqueous HCl (2 M, 10 mL) was added to quench the reaction. After extraction with ethyl acetate for three times, the organic phase was washed with brine, and then dried over anhydrous Na2SO4. After the solution was filtered and evaporated under vacuum, the residue was subjected to silica gel column chromatography (eluting with petroleum ether/ethyl acetate) to give the corresponding difluoromethylated carbinol 4a as a white solid (307.5 mg, 88%).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Article; Jiang, Fanzhou; Ni, Chuanfa; Hu, Jinbo; Journal of Fluorine Chemistry; vol. 198; (2017); p. 67 – 75;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com