4677-20-7, 4-(2-Bromoethyl)tetrahydropyran is a Tetrahydropyrans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Example 51 can be prepared according to method 14 with modifications known to one of ordinary skill in the art. The last step of the preparation is provided: A mixture of 4-(2- bromoethyl)tetrahydro-2H-pyran (12.54 mg, 0.065 mmol), (E)-l-(4-(5-carbamoyl-2-(l-ethyl-3- methyl-lH-pyrazole-5-carboxamido)-lH-benzo[d]imidazol-l-yl)but-2-en-l-yl)-2-(l-ethyl-3- methyl-lH-pyrazole-5-carboxamido)-7-hydroxy-lH-benzo[d]imidazole-5-arboxamide (45 mg, 0.065 mmol) and potassium carbonate (22.44 mg, 0.162 mmol) was heated for 3hr at 85 C in DMSO (650 muIota) and NMP (650 muIota), then cooled. The residue was purified via acidic reverse phase chromatography (5% to 50% in 0.1% TFA in MeCN to 0.1% TFA in water; 50x30mm Phenomenex Eclipse, 5muMu C18 column, 20 min gradient). The pure fractions were partitioned between EtOAc and aqueous saturated sodium bicarbonate, the organic layer was separated, dried over sodium sulfate and evaporated in vacuoXa provide the title compound (8mg, 15.3% yield) as a white solid. *H NMR (DMSO-cfe, 600MHz): delta (ppm) 12.83 (br s, 2 H), 7.97-8.00 (m, 1 H), 7.93 (br s, 2 H), 7.69 (dd, 7=8.4, 1.5 Hz, 1 H), 7.63 (s, 1 H), 7.41 (d, 7=8.3 Hz, 1 H), 7.33 (br d, 7=11.4 Hz, 2 H), 7.29 (s, 1 H), 6.55 (s, 1 H), 6.52 (s, 1 H), 5.96-6.02 (m, 1 H), (2225) 5.70-5.79 (m, 1 H), 4.93 (br d, 7=5.0 Hz, 2 H), 4.82 (br d, 7=5.3 Hz, 2 H), 4.49-4.58 (m, 4 H), 3.96 (br t, 7=6.7 Hz, 2 H), 3.75 (br dd, 7=11.2, 2.9 Hz, 2 H), 3.16-3.23 (m, 2 H), 2.12 (d, 7=12.7 Hz, 6 H), 1.50-1.53 (m, 1 H), 1.45-1.49 (m, 2 H), 1.43 (br d, 7=11.9 Hz, 2 H), 1.28 (m, 6 H), 1.08 (br dd, 7=12.0, 3.6 Hz, 2 H); LCMS (LCMS Method K): Rt = 0.90 min, [M+H]+ = 805.5.
4677-20-7, The synthetic route of 4677-20-7 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CHARNLEY, Adam Kenneth; DARCY, Michael G.; DODSON, Jason W.; DONG, Xiaoyang; HUGHES, Terry V.; KANG, Jianxing; LEISTER, Lara Kathryn; LIAN, Yiqian; LI, Yue; MEHLMANN, John F.; NEVINS, Neysa; RAMANJULU, Joshi M.; ROMANO, Joseph J.; WANG, Gren Z.; YE, Guosen; ZHANG, Daohua; (451 pag.)WO2017/175147; (2017); A1;,
Tetrahydropyran – Wikipedia
Tetrahydropyran – an overview | ScienceDirect Topics