4-Hydroxybenzamide synthesis
- Product Name:4-Hydroxybenzamide
- CAS Number:619-57-8
- Molecular formula:C7H7NO2
- Molecular Weight:137.14
99-96-7
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619-57-8
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Yield:619-57-8 98.7%
Reaction Conditions:
with 1,4-diaza-bicyclo[2.2.2]octane;methyl carbamate at 130 - 180; for 4.5 h;Temperature;
Steps:
1.1; 2.1; 3.1
1) In a 500ml reactor, add 139.6g of p-hydroxybenzoic acid, 90.7g of methyl carbamate, and 4.2g of triethylenediamine. Slowly increase the temperature to 130°C for 30 minutes, and then slowly increase the temperature to 180°C. React for 4 hours at the temperature. After the temperature reaches 180°C, the content of p-hydroxybenzoic acid will be detected. When the content of p-hydroxybenzoic acid is less than 0.1%, the reaction is considered complete. At this temperature, the reaction is completed in 4 hours. The product is P-Hydroxybenzamide; the liquid phase shows that the content is ≥99%. After the reaction is completed, the methyl carbamate and triethylenediamine are recovered by vacuum distillation to obtain 137.5 g of p-hydroxybenzamide white powder with a melting point of 161°C. The purity is 99.5% and the yield is 98.7% after liquid phase detection;
References:
CN112552207,2021,A Location in patent:Paragraph 0039-0041; 0045-0047; 0051-0053
5942-20-1
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