Method for producing 5-n-butyl-2-benzoglioxaline methyl carbamate
A technology of methyl benzimidazole carbamate and n-butylaniline, which is applied in the field of preparing 5-n-butyl-2-benzimidazole methyl carbamate, that is, parbendazole, can solve the problem of long reaction steps and difficulty in industrialization Production, high toxicity and other problems, to achieve the effect of mild reaction conditions, reduced production, high conversion rate
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example 1
[0020] In a 250mL four-necked flask equipped with a thermometer and a stirring device, add 30.81g (0.3021mol) of acetic anhydride (refined anhydrous) and a small amount of concentrated sulfuric acid, control the temperature at about 50°C, and dropwise add 15.0g (0.1007mol) For n-butylaniline, keep the reaction at 45-50°C for about 1 hour, then cool the reaction liquid, and then pour it into a large amount of ice-water mixture, white crystals will precipitate out, and use NaCO 3 The solution was washed until neutral, filtered with suction, and dried to obtain a crude product. Then recrystallize from n-heptane to obtain 16.62 g of p-n-butylacetanilide with a yield of 87.0%. Melting point: 104℃~105℃.
example 2
[0022] In a 250mL four-necked flask with a thermometer and a stirring device, add 51.36g (0.5035mol) of acetic anhydride (refined anhydrous) and a small amount of concentrated sulfuric acid, control the temperature at about 50°C, and drop 15.0g (0.1007mol) For n-butylaniline, keep the reaction at 45-50°C for about 1 hour, then cool the reaction liquid, and then pour it into a large amount of ice-water mixture, white crystals will precipitate out, and use NaCO 3 The solution was washed until neutral, filtered with suction, and dried to obtain a crude product. Then recrystallize from n-heptane to obtain 17.02 g of p-n-butylacetanilide with a yield of 88.5%. Melting point: 104℃~105℃.
example 3
[0024] In a 250mL four-neck flask equipped with a thermometer and a stirring device, add 61.63g (0.6078mol) of acetic anhydride (refined anhydrous) and a small amount of concentrated sulfuric acid, control the temperature at about 50°C, and dropwise add 15.0g (0.1007mol) Add n-butylaniline dropwise, keep the reaction at 50°C-55°C for about 1 hour, then cool the reaction solution, then pour it into a large amount of ice-water mixture, white crystals precipitate out, use NaCO 3 The solution was washed until neutral, filtered with suction, and dried to obtain a crude product. Then recrystallize from n-heptane to obtain 17.19 g of p-n-butylacetanilide with a yield of 90.0%. Melting point: 104℃~105℃.
[0025] Synthesis of 4-n-butyl-2-nitroacetanilide
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