ChemicalBook CAS DataBase List 4-Aminobenzamidine dihydrochloride

4-Aminobenzamidine dihydrochloride synthesis

5synthesis methods

Product Name:4-Aminobenzamidine dihydrochloride
CAS Number:2498-50-2
Molecular formula:C7H11Cl2N3
Molecular Weight:208.09

4-Aminobenzamididine dihydrochloride is obtained by cyanation, addition, amination and reduction of 4-nitrobenzoic acid.

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2498-50-2
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Yield:2498-50-2 97.8%

Reaction Conditions:

Stage #1:N-(4-cyanophenyl)acetamide with sodium amide in dimethyl sulfoxide at 20 - 80; for 1.5 h;Large scale;
Stage #2: with hydrogenchloride in ethanol;dimethyl sulfoxide; pH=3 - 4 at 0; for 1.5 h;Large scale;Solvent;Reagent/catalyst;Temperature;

Steps:

1 Example 1
Will 1kgAcetaminobenzonitrileSoluble5L dimethyl sulfoxide,853g sodium amide was added in batches.After stirring at room temperature for 30 minutes,The temperature was raised to 80 ° C and the reaction was continued for 1 hour.TLC monitoring (developing agent: ethyl acetate / petroleum ether (60 ~ 90 ° C) = 1 / 1 (V / V)) to para-acetamidobenzonitrile disappeared.The reaction solution was cooled to 0 ° C,Add concentrated hydrochloric acid to the system pH=3-4 with rapid stirring.After stirring for 30 minutes,5 L of absolute ethanol was added to the reaction solution.Stir for 1 hour,The reaction solution was added to 10 L of ethyl acetate.Stir at room temperature for 1 h,filter,The filter cake was dried under reduced pressure at 40 ° C for 4 hours.Obtained 1.27 kg of p-aminobenzonitrile hydrochloride,As a white solid,The yield is 97.8%.The purity is 99.6%.

References:

Sichuan Qing Mu Pharmaceutical Co., Ltd.;Li Xiaoxun;Hu Tongjun;Li Jianguo;Wang Bo;Wang Ying CN108752237, 2018, A Location in patent:Paragraph 0032; 0033; 0035; 0037; 0039; 0041; 0043; 0045

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