Electric Literature of 69113-59-3,Some common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, molecular formula is C7H4IN, 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.
General procedure: In an argon-filled glovebox, an oven-dried Schlenk tube equipped with a Teflon stir bar was charged with CuI (9.5 mg, 0.05 mmol, 5 mol%) followed by anhydrous toluene (2.0 ml), secondary phosphine (1.00 mmol), and L4 (49.54 mg, 0.30 mmol, 30 mol%). The solution was stirred for 5-10 min. Then the (hetero)aromatic bromide (1.00 mmol) and KOtBu (224.42 mg, 2.0 mmol) were added at once followed by anhydrous toluene/THF (0.5 mL/0.5 mL). The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 100 C for 24 h. The reaction mixture was then cooled to room temperature and filtered with dichloromethane to remove any insoluble residues. The filtrate was concentrated in vacuo; the residue was purified by flash chromatography on silica to obtain the analytically pure product (kept under argon).
The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Li, Chun-Jing; Lue, Jing; Zhang, Zhi-Xun; Zhou, Kun; Li, Yan; Qi, Guang-Hui; Research on Chemical Intermediates; vol. 44; 7; (2018); p. 4547 – 4562;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com