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ChemicalBook CAS DataBase List 2-Isopropyl-N,2,3-trimethylbutyramide

2-Isopropyl-N,2,3-trimethylbutyramide synthesis

3synthesis methods
N,2,3-Trimethyl-2-isopropylbutamide can be synthesized in activated PMA-SiO2 solid acid catalyst in water at 90 by methanol and 2,2-diisopropylpropionitrile.
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Yield:51115-67-4 95 %

Reaction Conditions:

Stage #1: N-methylpropanamidewith n-butyllithium in tetrahydrofuran at -40;Inert atmosphere;
Stage #2: isopropyl bromide in tetrahydrofuran at -40;Inert atmosphere;Temperature;

Steps:

1-10 Example 2

(1) Add 2mol of N-methylpropanamide (174.24g) to the dry three-neck bottle at -40 °C, 1300ml of dried tetrahydrofuran solution, add 2.4L of n-butyl lithium (2.5mol/L) dropwise to the reaction system under nitrogen protection, and obtain mixed solution A after dropping the reaction at the same temperature for 1 hour;(2) Add 4mol of 2-bromopropane (486g)-tetrahydrofuran mixture to the mixed solution A obtained in step (1), and drop the reaction at the same temperature for 1.5 hours;(3) After the completion of the detection reaction by gas chromatography, 3L of ammonium chloride solution (1mol/L) was added to the reaction system to quench the reaction, hydrochloric acid solution (2mol/L) was added to adjust the pH of the reaction system to 7, and then extracted by 6L ethyl acetate, and 327g of white solid was obtained after removing the solvent under reduced pressure , with a yield of 95% and a purity of 97%.

References:

CN115477593,2022,A Location in patent:Paragraph 0025-0065

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