N-substituted piperazine bismuth dicarbamate (Ⅲ) complex and its preparation method and application in the preparation of antitumor drugs
An anti-tumor drug, the technology of bismuth dicarbaminate, which is applied in the field of anti-tumor drugs, can solve the problems of single structure, low clinical application value, and few anti-tumor cell lines, and achieve wide application prospects, good anti-tumor activity, and significant inhibitory effect. The effect of tumor activity
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Embodiment 1
[0026] Example 1: 1-methylpiperazine bismuth dicarbamate and its preparation
[0027] Add 0.501g (5mmol) 1-methylpiperazine, 0.25g (6mmol) sodium hydroxide, and 15mL anhydrous methanol to a round-bottomed flask, stir and dissolve in a cold water bath at 0-5°C, then add dropwise 0.76g ( 10mmol) CS 2 , Low temperature magnetic stirring reaction for 2h, magnetic stirring reaction at room temperature for 4h.
[0028] 0.53g (1.7mmol) BiCl 3 Dissolve in 15 mL of anhydrous methanol, drop into the above reaction solution, stir at room temperature for 3 h, filter with suction, wash with anhydrous methanol, and dry in vacuo. The solid was recrystallized from dichloromethane and ethanol to obtain 0.85 g of a yellow powder solid, yield 69.4%, melting point: 197-199°C, number N058.
[0029] 1 HNMR (400MHz, CDCl 3 ),δ:2.326(9H,s,-CH 3 ),2.505~2.530(12H,t,N-CH 2 , J=4.8Hz), 4.131~4.155(12H,t,N-CH 2 ,J=4.8Hz).
[0030] Molecular formula: C 18 h 33 N 6 S 6 Bi, elemental analysis r...
Embodiment 2
[0031] Embodiment two: 1-ethylpiperazine bismuth dicarbamate and its preparation
[0032] Add 0.571g (5mmol) 1-ethylpiperazine, 0.25g (6mmol) sodium hydroxide, and 15mL anhydrous methanol to a round-bottomed flask, stir and dissolve in a cold water bath at 0-5°C, then add dropwise 0.76g ( 10mmol) CS 2 , Low temperature magnetic stirring reaction for 2h, magnetic stirring reaction at room temperature for 4h.
[0033] 0.53g (1.7mmol) BiCl 3 Dissolve in 15mL of anhydrous methanol, drop into the above reaction solution, and stir at room temperature for 4h. A yellow precipitate precipitated, was suction filtered, washed with anhydrous methanol, and dried. The solid was recrystallized from acetonitrile to obtain 1.15 g of a yellow solid with a yield of 88.8%. Melting point: 122-124°C, number N063.
[0034] 1 HNMR (400MHz, CDCl 3 ),δ:1.094~1.129(9H,t,-CH 3 , J=6.8Hz), 2.430~2.482(6H,q,-CH 2 ,J=6.8Hz),2.539~2.563(12H,t,N-CH 2 , J=4.8Hz), 4.135~4.159(12H,t,N-CH 2 ,J=4.8Hz). ...
Embodiment 3
[0036] Example three: 1-benzylpiperazine bismuth dicarbamate and its preparation
[0037] Add 0.881g (5mmol) 1-benzylpiperazine, 0.25g (6mmol) sodium hydroxide, and 15mL anhydrous methanol to a round-bottomed flask, stir and dissolve in a cold water bath at 0-5°C, then add dropwise 0.76g ( 10mmol) CS 2 , Low temperature magnetic stirring reaction for 2h, magnetic stirring reaction at room temperature for 4h.
[0038] 0.53g (1.7mmol) BiCl 3 Dissolve in 15 mL of anhydrous methanol, drop into the above reaction solution, stir at room temperature for 4 h, filter with suction, wash with anhydrous methanol, and dry in vacuo. The solid was recrystallized from dichloromethane-methanol to obtain 1.29 g of yellow crystals, yield 80.4%, melting point: 255-256°C.
[0039] 1 HNMR (400MHz, CDCl 3 ),δ:2.530~2.554(12H,t,N-CH 2 , J=4.8Hz), 3.529(6H,s,Ph-CH 2 ),4.098~4.122(12H,t,N-CH 2 , J=4.8Hz), 7.269~7.349 (15H, m, Ph-H, J=6.4-7.6Hz).
[0040] Molecular formula: C 36 h 45 N 6 S ...
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