51436-99-8, 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 51436-99-8 as follows.
Add sodium hydride (60% dispersion in oil, 880 mg, 22 mmol) to a solution OF 4- HYDROXY-L-METHYL-PIPERIDINE (2. 304 g, 20 mmol) in DMF (12 mL), stir. After 30 min., add 4-BROMO-2-FLUOROTOLUENE (4.159 g, 22 mmol) and heat at 70 C. After 21 hr. , quench the reaction with saturated NAHC03 solution, extract with ether three times, combine the organic layers, wash with saturated NaCl solution, dry over NA2SO4, filter and concentrate to give a residue. Purify by chromatography (silica gel, eluting with 6% 2M NH3- methanol in CH2CI2) provides of the title compound as a slightly yellow oil (3.90 g, 69%). Mass spectrum (ion spray): m/z = 284.0 (M ;’H NMR (CDCI3, ppm): 7.01 (m, 3H), 4.35 (m, 1H), 2.66 (m, 2H), 2.36 (m, 2H), 2.34 (s, 3H), 2.19 (s, 3H), 2.03 (m, 2H), 1.85 (m, 2H).
According to the analysis of related databases, 4-Bromo-2-fluorotoluene, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ELI LILLY AND COMPANY; WO2004/94380; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary