Bis(aminodithioformic acid)-1,3-propylene diester compound and its synthesis method, pharmaceutical composition and application
A technology of dimethylaminodithioformic acid and compounds, which is applied in the field of preparation of drugs for treating or preventing cancer, and can solve problems such as failure to function, tumor cell death, etc.
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Embodiment 1
[0120] Example 1: Bis(dimethylaminodithioformic acid)-2-acetyl-1,3-propanediester
[0121]
[0122] Dissolve dimethylamine hydrochloride (16.31g, 200mmol) in acetone (23.24g, 400mmol), add paraformaldehyde (7.21g, 240mmol), 50mL water and 5mL isopropanol, and reflux for 16h. After cooling to room temperature, it was directly used in the next step without separation and purification. Dissolve dimethylamine hydrochloride (32.62g, 400mmol) in 100mL of acetone, add triethylamine (80.96g, 800mmol), stir for 15min, add carbon disulfide (38.07g, 500mmol), react at room temperature for 30min, add the previous step The reaction solution was reacted at room temperature for 17h. The acetone in the reaction solution was distilled off under reduced pressure, the residue was extracted with ethyl acetate (40mL×3), the organic phases were combined, washed with saturated brine (30mL×2), dried over anhydrous sodium sulfate, filtered, concentrated, and the remaining The compound was recryst...
Embodiment 2
[0126] Example 2: Bis(dimethylaminodithioformic acid)-2-benzoyl-1,3-propanediester
[0127]
[0128] Dissolve acetophenone (0.61g, 5mmol) in 10mL of acetic acid, add dimethylamine hydrochloride (0.82g, 10mmol) and paraformaldehyde (0.31g, 10mmol), reflux for 12h, and cool the reaction solution to room temperature , The solvent was distilled off under reduced pressure to obtain intermediate 2a. Dissolve dimethylamine hydrochloride (0.82g, 10mmol) in 25mL of water, add potassium carbonate (2.77g, 20mmol), stir for 15min, add carbon disulfide (0.92g, 12mmol), react at room temperature for 30min, add intermediate 2a, After reacting at room temperature for 12 hours, a yellow solid precipitated out, was filtered with suction, washed with water, and dried. The solid was recrystallized from ethyl acetate to obtain 0.83 g of a light yellow solid, and the total yield of the two-step reaction was 43%.
[0129] 1 HNMR (400MHz, CDCl 3 ):δ=3.23(s,6H),3.45(s,6H),3.57-3.62(m,2H),3.67-3...
Embodiment 3
[0132] Example 3: Bis(dimethylaminodithioformic acid)-2-(4-fluorobenzoyl)-1,3-propanediester
[0133]
[0134] Using 4-fluoroacetophenone as a raw material, the synthesis method is the same as in Example 2, and the total yield of the two-step reaction is 27%.
[0135] 1 HNMR (400MHz, CDCl 3):δ=3.31(s,6H),3.52(s,6H),3.62-3.67(m,2H),3.72-3.77(m,2H),4.50(s,1H),7.11-7.15(m,2H ),8.12-8.16(m,2H).
[0136] 13 CNMR (100MHz, CDCl 3 ): δ=38.52, 41.60, 44.47, 45.39, 115.72(d, J=22Hz), 131.77(d, J=10Hz), 132.94, 166.08(d, J=254Hz), 196.21, 199.55.
[0137] Anal. CaldforC 16 h 21 FN 2 OS 4 : C, 47.50; H, 5.23; N, 6.92; Found: C, 47.75; H, 5.36; N, 7.03.
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