Substituted aryl methylene sulfonylated aza cyclo-pentanone compounds, its medicine compositions and its preparing process and use
A technology of arylmethylenesulfonyl nitrogen and heterocyclopentanone, which can be used in the field of medicine and can solve problems such as enzyme imbalance in the body and cardiovascular damage.
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Embodiment 1
[0034] Example 1: Preparation of (Z)-5-(3,5-di-tert-butyl-4-hydroxyphenylmethylene)-2-p-toluenesulfonimide-4-thiazolidinone (A1)
[0035] Add 2.34g (10mmol) 3,5-di-tert-butyl-4-hydroxybenzaldehyde, 1.16g (10mmol) 2-imino-4-thiazolidinone and 20ml water in a 50ml round-bottomed flask, and add 0.075 g (1 mmol) isopropanolamine. Reflux for 10 h, cool to room temperature, and filter with suction, wash the filter cake with cold water, and dry to obtain 2.69 g of yellow solid, mp 283-286°C, yield 81.0%. is (Z)-5-(3,5-di-tert-butyl-4-hydroxyphenylmethylene)-2-imino-4-thiazolidinone (intermediate A).
[0036] Dissolve 0.198g (0.6mmol) of the intermediate A in 10ml of dry tetrahydrofuran, and add 0.120g (1.2mmol) of triethylamine (1.2mmol) and 0.228g (1.2mmol) of p-toluenesulfonyl chloride while stirring. Reaction at 50°C for 12h, preparative thin layer separation, the developing solvent was dichloromethane:methanol=15:1, 0.102g of yellow solid was obtained, mp 264-267°C, yield 35.0%...
Embodiment 2
[0037] Example 2: Preparation of (Z)-5-(3,5-di-tert-butyl-4-hydroxyphenylmethylene)-2-benzenesulfonimide-4-thiazolidinone (A2)
[0038] Carry out by the method for embodiment 1.
[0039] The intermediate A is obtained first, the raw materials used in the condensation reaction are 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-imino-4-thiazolidinone, and the catalyst is ethanolamine.
[0040] The reagent used in the sulfonylation process is benzenesulfonyl chloride, and the basic catalyst used is dimethylaminopyridine.
[0041] The product A2(Z)-5-(3,5-di-tert-butyl-4-hydroxyphenylmethylene)-2-benzenesulfonimido-4-thiazolidinone was obtained as a yellow solid, mp 252 -255°C, yield 18.9%.
Embodiment 3
[0042] Example 3: Preparation of (Z)-5-(4-hydroxyphenylmethylene)-2-benzenesulfonylimide-3-benzenesulfonyl-4-thiazolidinone (A3)
[0043] The same method as in Example 1 was used.
[0044] First synthesize (Z)-5-(4-hydroxyphenylmethylene)-2-imino-4-thiazolidinone, the raw materials used are 4-hydroxybenzaldehyde and 2-imino-4-thiazolidine Ketones, the catalyst is isopropanolamine. A yellow solid was obtained, mp > 300°C, and the yield was 82.4%.
[0045] The reagent used in the sulfonylation process is benzenesulfonyl chloride, and the basic catalyst used is pyridine.
[0046] The product A3 was obtained as light yellow solid, mp 222-226°C, yield 22.5%.
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