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 2318-25-4 as follows. COA of Formula: C7H14ClNO3
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 2318-25-4 as follows. COA of Formula: C7H14ClNO3
To anhydrous ethanol (460 g, 10.0 mol) at -3O0C was bubbled in anhydrous hydrogen chloride until the total weight of 821 g of etaCl/EtOeta solution (44percent (w/w) was obtained.Ethyl cyanoacetate (452 g) was added into the etaCl/EtOeta solution (292 g), the mixture was cooled to ice-salt bath temperature and stirred for 1 hours. The reaction was warmed to room temperature and stood overnight. A white precipitate of 102 was obtained and this mixture was used directly in the next step.The obtained mixture was added to a mixture of ether and a solution OfK2COs (828 g) in water (2500 mL). The ether layer was separated, dried over Na2SO4, and filtered. The filtrate was concentrated under reduced pressure to give compound 103 (445 g) as a colorless oil.A mixture of compound 103 (445 g) and ammonium chloride (149.5 g) in ethanol (1500 mL) was heated to reflux for 8 h. The solid was isolated and the filtrate was concentrated. The residue was washed with ether and acetone to give product 104 (220 g, 33percent total yield in three steps). LCMS: 131 [M+l]+, 1H NMR (DMSO-J6): delta 1.22 (t, J= 6.9 Hz, 3H), 3.68 (s, 2H), 4.16 (q, J= 6.9 Hz, 2H), 9.04 (s, 2H), 9.32 (s, 2H).
According to the analysis of related databases, 2318-25-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; CURIS, INC.; WO2008/33747; (2008); A2;,
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