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ChemicalBook CAS DataBase List Mefenacet
73250-68-7

Mefenacet synthesis

4synthesis methods
-

Yield:73250-68-7 98%

Reaction Conditions:

Stage #1:2(3H)-Benzothiazolone with sodium hydroxide
Stage #2:N-methyl-2-chloroacetanilide with sodium hydroxide in N,N-dimethyl-formamide at 50; for 4 h;Solvent;Reagent/catalyst;Temperature;

Steps:

1.2; 2-6 (2) Preparation of Mefenacet:
First, 151.2 mg (1.0 mmol) of benzothiazolone solid powder was added to 15percent sodium hydroxide aqueous solution (the amount of sodium hydroxide was 80 mg, 2.0 mmol), and stirred until all the benzothiazolone powder was dissolved to obtain benzothiazolone. Sodium thiazolone solution, the reaction formula is as follows:Then measure 4mL of DMF (N,N-dimethylformamide) with a graduated cylinder, add 275.5mg (1.5mmol) of 2-chloro-N-methyl-N-phenylacetamide to DMF, and stir to obtain a clear and transparent Brown 2-chloro-N-methyl-N-phenylacetamide solution;Finally, the 2-chloro-N-methyl-N-phenylacetamide solution was added to the sodium benzothiazolone solution, stirred thoroughly and mixed uniformly, and heated to reflux for 4 hours at 50°C. After the reaction was stopped, the reaction Add dilute hydrochloric acid to the solution to adjust the pH of the reaction solution to neutral; extract the reaction solution with dichloromethane, collect the organic phase, dry the organic phase with anhydrous magnesium sulfate, then filter and concentrate to obtain a concentrated solution;Using DMF as a benign solvent and water as a poor solvent (the volume ratio of DMF to water is 1:5), the concentrated solution was recrystallized to obtain 292.4 mg of white crystals of mefenacet with a yield of 98.0percent. The reaction formula is as follows:

References:

Inner Mongolia University of Technology;Zhu Ning;Hong Hailong;Han Limin CN111303073, 2020, A Location in patent:Paragraph 0023; 0026-0028; 0030-0065

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