Reference of 630-17-1, 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 630-17-1 as follows.
(0317) Obtained according to the general method described previously. (0318) Reagents: 3-(2,6-Difluorophenyl)-8-methyl-4-oxo-2-thioxo-1,2,3,4-tetrahydroquinazoline (0.32 mmol, 0.097 g), neopentyl bromide (0.64 mmol, 0.080 mL), K2CO3 (0.0045 g). (0319) The reaction conditions were: 12 hours at ambient temperature. (0320) Purification was carried out by means of silica gel column chromatography (hexane/ethyl acetate, in a ratio of 6:1 by volume). (0321) The yield obtained was: a white solid (51 mg, 42%). P.f.: 152.3 C. 1H-RMN (400 MHz, DMSO) delta: 7.94 (dd, 1H, J=7.9, 0.8 Hz), 7.81-7.73 (m, 2H), 7.49-7.40 (m, 3H), 3.34 (s, 2H), 2.60 (s, 3H), 0.95 (s, 9H). 13C-RMN (100 MHz, DMSO) delta: 160.7, 158.8 (d, 2C, J=252.2 Hz), 156.0, 145.9, 136.9, 135.1, 134.1, 126.9, 125.1, 118.8, 113.5, 44.9, 32.6, 28.9, 17.6, purity analysed by HPLC >99%. EM (m/z): 375 [M+H
According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Consejo Superior De lnvestigaciones Cientificas (CSIC); Martinez Gil, Ana; Gil Ayuso-Gontan, Carmen Belen; Perez Fernandez, Daniel Ignacio; Garcia Fernandez, Ana Maria; (22 pag.)US2016/340320; (2016); A1;,
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