Synthesis method of 4-Hydroxythiobenzamide
A technology of hydroxythiobenzamide and hydroxybenzamide, which is applied in the field of synthesis of p-hydroxythiobenzamide, can solve the problems of difficult industrialization and low processing costs, achieve low cost, easy operation, and realize industrial production Effect
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Embodiment 1
[0030] Put 150mL of 28% concentrated ammonia water and 8.6g (0.060mol) of methyl p-hydroxybenzoate in the reaction kettle. Under the condition of stirring, control the temperature at 100-120°C and keep it warm for the reaction. TLC detection shows that the reaction is complete. Concentrate the final reaction solution in a rotary evaporator to twice the amount of the feed, filter and dry to obtain a white solid that is p-hydroxybenzamide 7.63g (0.055mol), yield rate 97.8%, HPLC purity 99.1%
Embodiment 2
[0032] Put 150mL of 28% concentrated ammonia water and 8.6g (0.060mol) of methyl p-hydroxybenzoate in the reaction kettle. Under the condition of stirring, control the temperature at 100-120°C and keep it warm for reaction. TLC detection shows that the reaction is complete. Concentrate the final reaction solution in a rotary evaporator to 1.5 times the amount of feed, and then separate and dry by suction filtration to obtain a white solid that is p-hydroxybenzamide 7.64g (0.056mol), yield 98.0%, HPLC purity 96.3%.
Embodiment 3
[0034] Put 100mL of 28% concentrated ammonia water and 8.6g (0.060mol) of methyl p-hydroxybenzoate in the reaction kettle. Under the condition of stirring, control the temperature at 100~120°C and keep the reaction. TLC detects that the reaction is complete. Concentrate the final reaction liquid in a rotary evaporator to twice the amount of feed, and then separate and dry by suction filtration to obtain 7.54 g (0.055 mol) of white solid p-hydroxybenzamide, with a yield of 96.7% and a purity of 97.2% by HPLC.
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