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. 3616-56-6, name is 2,2-Diethoxy-N,N-dimethylethanamine, A new synthetic method of this compound is introduced below., Quality Control of 2,2-Diethoxy-N,N-dimethylethanamine
Example 2 (E)-4-Dimethylamino-But-2-Enoic acid-[4-(3-Chloro-4-Fluoro-Phenylamino)-7-((S)-Tetrahydrofuran-3-Yloxy)-Quinazolin-6yl]-Amide 5.6 litres of 30percent hydrochloric acid (53.17 mol) are added to 4.4 litres of water. Then 4.28 kg of 95percent (dimethylamino)-acetaldehyde-diethylacetal (26.59 mol) are added dropwise within 20 minutes at 30° C. The reaction solution is stirred for 8 hours at 35° C. stirred, cooled to 5° C. and stored under argon. This solution is referred to as solution B. 4.55 kg (68.06 mol) of potassium hydroxide are dissolved in 23.5 litres of water and cooled to -5° C. This solution is referred to as solution C. 5.88 kg (10.63 mol) of diethyl ((4-(3-chloro-4-fluoro-phenylamino)-7-(tetrahydrofuran-3-yloxy)-quinazoline-6-ylcarbamoyl)-methyl)-phosphonate and 0.45 kg of lithium chloride (10.63 mol) are placed in 23.5 litres of tetrahydrofuran and cooled to -7° C. The cold solution C is added within 10 minutes. Then solution B is added at -7° C. within 1 hour. After stirring for a further hour at -5° C. the reaction mixture is heated to 30° C. and combined with 15 litres of water. After cooling to 3° C. the suspension is suction filtered, the precipitate is washed with water and dried. Yield: 5.21 kg of crude product, 100percent, water content: 6.7percent The crystallisation of the crude product is carried out with butyl acetate/methylcyclohexane Yield: 78percent purity HPLC 99.4Fl percent, water content 5.4percent
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; Boehringer Ingelheim International GmbH; US2005/85495; (2005); A1;,
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