Preparation method of 2-methoxy-5-sulfamoylbenzoic acid
A technology of sulfonamidobenzoic acid and methoxybenzenesulfonamide, which is applied in the field of preparation of 2-methoxy-5-sulfonamidobenzoic acid, and can solve problems such as physical and environmental impacts and rare synthetic methods , to achieve the effect of improving selectivity, moderate price, and mild reaction conditions
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Embodiment 1
[0023] A preparation method of 2-methoxy-5-sulfonamidobenzoic acid, comprising the following steps:
[0024] (1) Add 187 g (1.0 mol) of 4-methoxybenzenesulfonamide, 10.29 g of iron powder, 88 g (1.1 mol) of bromine and 2618 g of methylene chloride into the reactor, and heat up to 60 °C under stirring , reacted at this temperature for 6 h, naturally cooled to room temperature after the reaction was completed, filtered, and the filtrate was evaporated to remove the solvent under normal pressure to obtain 223.44 g of the crude product of 3-bromo-4-methoxybenzenesulfonamide, with a yield of 84.0%;
[0025] (2) Add 266 g (1.0 mol) of 3-bromo-4-methoxybenzenesulfonamide prepared in step (1), 13.3 g of cuprous iodide, and 180 g of cuprous cyanide (2.0 mol) and 2128 g of N,N-dimethylformamide, heated to 120°C under stirring conditions, reacted at this temperature for 12 h, cooled naturally to room temperature after the reaction, filtered, evaporated the filtrate to remove the solvent ...
Embodiment 2
[0033] Other steps are the same as in Example 1, except that the preparation method of 3-bromo-4-methoxybenzenesulfonamide in step (1) is as follows:
[0034] 187 g (1.0 mol) of 4-methoxybenzenesulfonamide, 8.42 g of iron powder, 80 g (1.0 mol) of bromine and 748 g of dichloromethane were added to the reactor, and the temperature was raised to 40 °C under stirring conditions. Reaction at high temperature for 4 h, naturally cooled to room temperature after the reaction, filtered, and the filtrate was evaporated to remove the solvent under normal pressure to obtain 198.97 g of 3-bromo-4-methoxybenzenesulfonamide crude product, the yield was 74.8%, and it was detected by HPLC The content is 99.21%, and the product can be directly used in the next reaction without further purification.
Embodiment 3
[0036]Other steps are the same as in Example 1, except that the preparation method of 3-bromo-4-methoxybenzenesulfonamide in step (1) is as follows:
[0037] Add 187 g (1.0 mol) of 4-methoxybenzenesulfonamide, 9.35 g of iron powder, 84 g (1.05 mol) of bromine and 1683 g of dichloromethane into the reactor, and raise the temperature to 50 °C under stirring conditions. Reaction at high temperature for 5 h, naturally cooled to room temperature after the reaction was completed, filtered, and the filtrate was evaporated to remove the solvent under normal pressure to obtain 206.42 g of 3-bromo-4-methoxybenzenesulfonamide crude product, yield 77.6%, detected by HPLC The content is 99.13%, and the product can be directly used in the next reaction without further purification.
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