Related Products of 628-77-3, 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 628-77-3 as follows.
Example 1.12: Preparation of 2′,3′,4′,4a’,5′,6′-hexahydro-l’/ -spiro[cyclohexane-l,7′- naphtho[l,8-cd]azepine] (Compound 117) Step A: Preparation of 3′,4′-dihyd ‘/ -spiro[cyclohexane-l,l’-naphthalen]-2′-one To a suspension of 60% sodium hydride dispersion (1.2 g, 30.00 mmol) in 70 mL THF, a solution of 3,4-dihydronaphthalen-2(lH)-one (2.0 g, 13.68 mmol) in 30 mL THF was added (over ca. 5 min). After stirring at room temperature for 10 min, 1,5-diiodopentane (2.04 mL, 13.71 mmol) was added. After stirring at room temperature overnight, the mixture was partly concentrated and residue was extracted with water and AcOEt. Organic phase was dried over MgS04, filtered, and concentrated. The residue was purified by biotage column chromatography (S1O2, hexane/ AcOEt gradient) to give 3′,4′-dihydro-2’H-spiro[cyclohexane-l,r-naphthalen]-2′-one (2.24 g, 76%) as a colorless oil. NMR (400 MHz, CDCI3) delta 1.27-1.39 (m, 1H), 1.62-1.79 (m, 7H), 2.10-2.17 (m, 2H), 2.70 (t, / = 7.1 Hz, 2H), 3.19 (t, / = 7.2 Hz, 2H), 7.12 (m, 2H), 7.22-7.27 (m, 1H), 7.38-7.40 (m, 1H).
According to the analysis of related databases, 628-77-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ARENA PHARMACEUTICALS, INC.; LEHMANN, Juerg; FEICHTINGER, Konrad; REN, Albert S.; SEMPLE, Graeme; (205 pag.)WO2017/23679; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com