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ChemicalBook CAS DataBase List 1-Benzyl-3-pyrrolidinone
775-16-6

1-Benzyl-3-pyrrolidinone synthesis

7synthesis methods
-

Yield:775-16-6 96%

Reaction Conditions:

with potassium etoxide in toluene at 30;Cooling;

Steps:

1.2; 1.2.1-1.2.3 2) prepare 1-benzyl-3-pyrrolidone solution;

(1) P1 liquid and toluene are pumped into the reaction tank with a vacuum pump, and the interlayer is passed through cooling water, and sodium ethylate is added under stirring, and the control temperature is between 20-30 °C, and the 25-30 °C of insulation reaction is completed for 3-4 hours after feeding; (2) above-mentioned clarification reaction solution is pumped into the reaction tank that has been added with purified water, hydrochloric acid, after the pumping finishes, stir for 5-10 minutes, the pH in the measuring tank should be 2-3, if not, add hydrochloric acid to adjust the pH to 2-3, stir for 5-10 minutes, stand still for 1-1.5 hours, put the lower layer aqueous solution into a turnover barrel or a reaction tank for temporary storage (the upper layer solution is pumped into another reaction tank for distillation). Then pump the aqueous solution in the turnover barrel into the reaction tank, start stirring, heat up and steam out the toluene aqueous solution, keep the temperature at 98-100 for 4.5 hours, and cool it to 50-60 through cooling water; (3) adjust pH to 8-10 with saturated aqueous sodium hydroxide solution, adjust pH to 8-9 with a small amount of glacial acetic acid, let stand for 5-6 hours, put the lower layer into a chemical sewage pipeline, and put the upper layer into a bucket to obtain 1-benzyl-3-pyrrolidone solution, weighed as a repeating nucleus, the filling material card is pending inspection; Material added mass ratio: benzyl-(3-ethoxy-3-enyl)-(1-vinylethoxymethyl)amine:toluene:sodium ethoxide:purified water in a ratio of 1:1:0.28:1:1.5; The yield of the 1-benzyl-3-pyrrolidone was 96%; The yield of 1-benzyl-3-pyrrolidone is the theoretical yield of 1-benzyl as benzyl-(3-ethoxy-3-enyl)-(1-vinylethoxymethyl)amine calculated based on the amount of base-3-pyrrolidone;

References:

CN114369052,2022,A Location in patent:Paragraph 0017; 0072-0073; 0087-0090

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