Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-1,3-diol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Safety of 3-Methylbutane-1,3-diol, blongs to alcohols-buliding-blocks compound. Safety of 3-Methylbutane-1,3-diol
To a solution of ethyl (2E) -3- (2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4-hydroxyphenyl) acrylate (10.0 g) in tetrahydrofuran (300 ml) were added tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1, 1′ – (azodicarbonyl) dipiperidine (9.7,6 g) , and the mixture was stirred overnight at 500C. Then, tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1,1′- (azodicarbonyl) dipiperidine (9.76 g) were added, and the mixture was stirred at 500C for 1 hr. The reaction mixture was concentrated, the obtained solid was washed with diisopropyl ether, and the filtrate was concentrated. The obtained residue was subjected to basic silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 45:55, v/v). The obtained residue was subjected to silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 3:7, v/v) to give ethyl (2E) -3- [2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4- (3-hydroxy-3- methylbutoxy) phenyl] acrylate (Reference Example 264) (1.46. g, yield: 12-%) ,as a pale-yellow solid. Recrystallization from ethyl acetate-hexane gave white crystals as 0.5 hydrate, melting point 63.5-66.00C.Then, ethyl (2E) -3- [2-{ [3-chloro-5-(trifluoromethyl) pyridin-2-yl] oxy}-4- (3-hydroxy-l, 1- dimethylpropoxy) phenyl] acrylate (Reference Example 265) (0.71 g, yield: 6%) was obtained as an orange oil.1H-NMR (300 MHz, DMSO-ds)delta: 1.20 (3 H, t, J = 7,2 Hz), 1.32 (6 H, s), 1.87 (2 H, t, J = 7.5 Hz), 3.55 – 3.62 (2 H, m) , 4.12 (2 H, q, J = 7.2 Hz), 4.40 (1 H, t, J = 5.4 Hz), 6.57 (1 H, d, J = 16.2 Hz), 6.96 (1 H, s) , 6.94 – 6.99 (1 H, m) , 7.55 (1 H, d, J = 16.2 Hz), 8.50 – 8.50 (1 H, m) , 8.63 (1 H, d, J = 2.0 EPO
At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.
Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/18314; (2007); A2;,
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