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. 59528-27-7, name is (4-Iodophenyl)methanamine hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: C7H9ClIN
A mixture of (4-iodophenyl)methanamine hydrochloride (2.64 g, 9.80 mmol, 1.0 eq), (lS,2S)- Nl,N2- dimethylcyclohexane-l, 2-diamine (0.31 mL 1.96 mmol, 0.2 eq), Sodium ascorbate (198 mg, 0.98 mmol, 0.1 eq), Copper Iodide (279 mg, 1.47 mmol, 0.15 eq), Sodium azide (1.27 g, 19.59 mmol, 2.0 eq) , Et3N (1.64 mL, 11.75 mmol, 1.2 eq) and 3-(prop-2-yn-l-yloxy)oxetane (9, 1.10 g, 9.80 mmol, 1.0 eq) in Methanol (24 mL) and water (6 mL) were purged with Nitrogen for 5 minutes and heated to 55 C for over night. The reaction mixture was cooled to room temperature and filtered through a plug of Celite and rinsed with Methanol (3 x 50 mL). Celite was added to the filtrate and the solvent was removed under reduced pressure. The residue was purified over silica gel (120 g) using dichloromethane/(methanol containing 12 % (v/v) aqueous ammonium hydroxide) as mobile phase. The concentration of (methanol containing 12 % (v/v) aqueous ammonium hydroxide) was gradually increased from 0 % to 25 % to afford (4-(4- ((oxctan-3-yloxy)mcthyl)-l //-l ,2,3-triazol- 1 -yl)phcnyl)mcthanaminc (32, 1.43 g, 56%) as an oil. LCMS m/z: [M + H]+ Calcd for C13H16N4O2 261.1346; Lound 261.1342.
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:
Patent; SIGILON THERAPEUTICS, INC.; SMITH, Devyn, McKinley; PERITT, David; VEISEH, Omid; HEIDEBRECHT, Richard; MILLER, Robert, James; (173 pag.)WO2019/195056; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com