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ChemicalBook CAS DataBase List 1-DIETHYLAMINO-3-BUTANONE

1-DIETHYLAMINO-3-BUTANONE synthesis

8synthesis methods
-

Yield: 65%

Reaction Conditions:

with hydrogenchloride in methanol at 100; for 30 h;Large scale;Mannich Aminomethylation;Concentration;

Steps:

1 Example 1, Preparation of 4-(N,N-diethyl)amino-2-butanone
Add 13.5 kg of diethylamine hydrochloride (compound A-1), 60 L of acetone, 4.8 kg of paraformaldehyde, 6 L of methanol, and 150 mL of concentrated hydrochloric acid into the reaction kettle; the reaction mixture was heated to 100°C and stirred for 30 Hour; the reaction solution is cooled down and spin-evaporated to remove the organic solvent; the resulting residue is added with sodium hydroxide solution to adjust the pH to 10-11, extracted with methyl tert-butyl ether, washed with organic phase, dried over anhydrous sodium sulfate, filtered, and filtrate Concentrate and dry in vacuo to give the compound 4-(N,N-diethyl)amino-2-butanone (A-2a) as a pale yellow oil (11.6 kg yield 66%). It was directly used in the next reaction without purification.

References:

Chengdu Normal College;He Bing;Feng Qiang;Sun Qidong;Wang Huan;Chen Le;Li Jiagen;He Yingsen;Zhang Xiaoling;Li Zhonghui CN111116446, 2020, A Location in patent:Paragraph 0124-0126; 0173-0177

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