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ChemicalBook CAS DataBase List 3-Aminobenzonitrile

3-Aminobenzonitrile synthesis

9synthesis methods
-

Yield:2237-30-1 91.3%

Reaction Conditions:

with thionyl chloride in toluene at 90 - 100;Temperature;Solvent;

Steps:

2; 5-6 Example 2:
Dehydration: Add 510g of toluene to a 1000ml reaction bottle with a brine-cooled reflux device,102g (0.75mol) of 3-aminobenzamide,Warm up to 90-100,Slowly add 205g (1.72mol) of sulfoxide chloride,There is a lot of exhaust gas (HCl+SO2),After the sulfoxide chloride drops,Continue to keep the heat until the materials are completely dissolved and no exhaust gas is released.Cool to 5060Is the dehydration solution,Keep warm.Hydrolysis: Add 102g water to a 1000ml reaction bottle,Stir to warm up to 50-60,Add the dehydration solution above,At this time, exhaust gas is generated (SO2),Control the drop acceleration,After dripping and stirring until no tail gas is released,While hot, adjust the pH of the water layer to 6.5-7.5 with 30% sodium hydroxide solution.Stand still and layer,The organic layer was slowly stirred and cooled to 0-5°C,filter,Appropriate amount of toluene washing at 0-5,80.8g of 3-aminobenzonitrile was obtained after drying,The yield was 91.3%, and the GC purity was 99.6%.

References:

Xinxiang Jin Yuan Chemical Co., Ltd.;Wang Zhusheng;Zhong Zhikui;Zhao Weikai;Zhou Mingyao;Tang He CN111269144, 2020, A Location in patent:Paragraph 0024-0026; 0033-0038

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