Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4640-66-8, name is 4-Chlorophenacylcyanide, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H6ClNO
with morpholine This substance has been prepared using morpholine as the activating partner (eg. WO 2015/156601, WO 2015/131113, Angewandte Chemie, International Edition (2013), 52, 14060-14064, Journal of Biological Chemistry (2012), 287, 28840-28851, WO2011/143660, Nature (2010), 468, 1067-1073 & US 6323214) or with diethylamine (WO 2009/063301). In all reports, the product was purified by chromatography followed by recrystallization and no mention of the ethyl-isomer as side product has been recorded ever anywhere.Purification via oxalate saltCrude aminothiophene (5.0 g, 19 mmol) and oxalic acid (1.7 g, 1 eq.) were taken up in methanol (50 ml). The light orange suspension was heated to reflux creating a dark red solution which then was cooled to ambient temperature. The brown suspension that formed was evaporated on a rotovap at 45 C/250-25 mb and the crude oxalate salt dried for 4 h at 45 C/25 mbar providing a yellow-orange crystalline solid (6.2 g, GC: 87% product, 13% ethyl isomer). a) The oxalate salt (3.0 g) was taken up in acetonitrile (30 ml, lOx v/w) and the brown suspension was heated to reflux. The red solution produced was cooled and stirred at 25 C/1 h. A brown suspension arose which was filtered and the purified product was washed with dichloromethane (4 ml). The salt recovered was dried at 45 C/25 mb for 3 h and the filtrate evaporated.Yield: 1.4 g yellow solid GC (area): 99% product, 1% ethyl isomer
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BLISS, Fritz; DU, Xiaohua; HE, Dawei; HILDBRAND, Stefan; SPURR, Paul; YE, Wenfa; ZHENG, Jianbing; (38 pag.)WO2018/109053; (2018); A1;,
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