4-azo salicylic acid derivative and process for producing the same and uses
A technology of azosalicylic acid and aminosalicylic acid is applied in the field of 4-azosalicylic acid derivatives and their preparation, and can solve the problems of unreachable treatment purpose, low colon concentration and the like
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Embodiment 1
[0091] Embodiment 1, a kind of 4-azosalicylic acid derivative
[0092]
[0093] Among them: R stands for:
[0094] R=—COOH,——NO 2 ,—CN,—H,—CHO,—CH 3 ,—OCH 3 ,—F,—Cl,—Br,—I,—CONHCH 2 COOH.
[0095] The preparation steps are:
[0096] A method for preparing 4-azosalicylic acid derivatives, the steps are,
[0097] One, the synthesis of 4-(N-benzyloxyformyl) aminosalicylic acid,
[0098] 4-Aminosalicylic acid (4-ASA) is started, first added to a saturated sodium bicarbonate solution under alkaline conditions to form a uniform suspension, then added dropwise with benzyl chloroformate, stirred in an ice bath for 10 hours to react, and reacted After the end, filter, wash the filtrate with ether (three times), discard the ether layer, adjust the pH value of the solution to acidity, produce off-white solid matter, extract three times with ethyl acetate, combine the organic phases, add desiccant to dry, and organic The phase was evaporated to dryness under reduced pressure to...
Embodiment 2
[0108] Embodiment 2: the steps are the same as in Example 1, specifically in step 1, stirring in an ice bath for 12 hours, the filtrate was washed five times with ether, extracted five times with ethyl acetate,
[0109] In step 2, stir the reaction for 36 hours
[0110] In step 3, the pressure in the autoclave is 0.4MPa and the time is that catalytic hydrogenation reaction occurs under 10 hours
[0111] In step 4, continue to react for 1.5 hours after dropping
[0112] In step 6, acetone-methanol (volume ratio 1:1), alkaline pH=10-11 conditions (potassium hydroxide solution can be used), hydrolysis reaction (time within 2 hours).
Embodiment 3
[0114] The steps are the same as in Example 1, specifically in step 1, stirring in an ice bath for 10 hours, washing the filtrate once with ether, and extracting once with ethyl acetate,
[0115] In step 2, stir the reaction for 48 hours
[0116] In step 3, the pressure in the autoclave is 0.6MPa and the time is that catalytic hydrogenation reaction occurs under 15 hours
[0117] In step 4, continue to react for 2 hours after dropping
[0118] In step 6, acetone-methanol (volume ratio 3:1), alkaline pH=10-11 conditions (can be sodium hydroxide solution), hydrolysis reaction (time within 6 hours).
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