Related Products of 4415-82-1 , The common heterocyclic compound, 4415-82-1, name is Cyclobutylmethanol, molecular formula is C5H10O, its 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.
Example 62A 3-(Cyclobutyloxy)pyridine hydrochloride With ice cooling, 2.59 g (13.7 mmol) of triphenylphosphine were added to a solution of 1.00 g (10.5 mmol) of 3-hydroxypyridine and 1.3 ml (13.7 mmol) of cyclobutylmethanol in 20 ml of THF, and the mixture was stirred for 5 min. 2.7 ml (13.7 mmol) of diisopropyl azodicarboxylate were then added dropwise and the reaction mixture was warmed to RT overnight. For work-up, water was added and the mixture was extracted twice with in each case 50 ml of ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated. The crude product was stirred with 50 ml of cyclohexane and the white solid was filtered off with suction and washed three times with in each case 20 ml of cyclohexane. The filtrate was concentrated and dissolved in 40 ml of diethyl ether, and 3 ml (12 mmol) of a 4N solution of hydrogen chloride in dioxane were added with ice cooling. The resulting beige precipitate was filtered off, washed twice with in each case 20 ml of diethyl ether and dried under HV. This gave 1.67 g (76% of theory) of the target compound. LC-MS [Method 10]: Rt=1.46 min; MS (ESIpos): m/z=164 (M+H)+ 1H-NMR (400 MHz, DMSO-d6): delta [ppm]=1.77-2.01 (m, 4H), 2.03-2.17 (m, 2H), 2.68-2.84 (m, 1H), 4.19 (d, 2H), 7.90 (dd, 1H), 8.10 (dd, 1H), 8.47 (d, 1H), 8.65 (d, 1H).
The synthetic route of 4415-82-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Bayer Pharma Aktiengesellschaft; BECKER-PELSTER, Eva Maria; BUCHGRABER, Philipp; BUCHMUeLLER, Anja; ENGEL, Karen; GNOTH, Mark Jean; HIMMEL, Herbert; KAST, Raimund; KELDENICH, Joerg; KLAR, Juergen; KNORR, Andreas; LANG, Dieter; LINDNER, Niels; SCHMECK, Carsten; SCHOHE-LOOP, Rudolf; TINEL, Hanna; TRUeBEL, Hubert; WUNDER, Frank; (97 pag.)US2016/318866; (2016); A1;,
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