Diaryl thioether compound, preparation method and antitumor application thereof
A compound and tumor technology, applied in the direction of thioether preparation, antineoplastic drugs, active ingredients of heterocyclic compounds, etc., can solve problems such as poor water solubility
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Embodiment 1
[0075] Preparation of O-ethyl-S-(3,4,5-trimethoxyphenyl)dithiocarbonate (ZLM-1)
[0076]
[0077] Dissolve 3,4,5-trimethoxyaniline (22.3g) in 30.5mL of concentrated hydrochloric acid and 250mL of water, cool in an ice bath to about 0°C, slowly add NaNO dropwise under stirring 2 Aqueous solution (9.2g), temperature controlled not to exceed 5°C, continued reaction for 15min after dropping, then added AcONa (20.0g). Slowly add this diazonium salt solution dropwise to KS at about 80°C 2 In COEt aqueous solution (48.7g dissolved in 120mL water), react at 70-80°C for 1h. After the reaction was completed, cool to room temperature, extract 100 mL×3 with EA, and combine the organic phases. Then dry with anhydrous sodium sulfate. After suction filtration, the filtrate was obtained, and the solvent was spun off to obtain 30.4 g of a reddish-brown oil, which was separated on a silica gel column to obtain 11.8 g of light yellow-white viscous solid, with a yield of 34%. 1 H NMR (400M...
Embodiment 2
[0079] Preparation of 3,4,5-trimethoxy-1-[(3-amino-4-nitrophenyl)thio]benzene (ZLM-2)
[0080]
[0081] Dissolve O-ethyl-S-(3,4,5-trimethoxyphenyl)dithiocarbonate ZLM-1 (4.0g) in THF (66mL), slowly add LiAlH4 (2.11g ), refluxed for 1 h, cooled to room temperature, adjusted to pH = 5 with 10% HCl, then extracted 100 mL×3 with EA, combined the organic phases, dried with anhydrous sodium sulfate for 1 h, and then filtered with suction to obtain the filtrate, which was spun off from the solvent. In 3,4,5-trimethoxythiophenol. Under nitrogen protection, K 2 CO3 (5.8g) and 5-chloro-2-nitroaniline (1.2g) were added to a 50mL two-necked flask, and then the 3,4,5-trimethoxythiophenol obtained in the previous step was dissolved in DMF (23.7mL) Add it into the reaction flask, reflux at 120°C, and monitor by TLC (developing solvent: PE:EA=4:1). The raw materials disappeared, the reaction was stopped, cooled to room temperature, diluted with 200 mL of water, extracted with EA (200 mL...
Embodiment 3
[0083] Preparation of 3,4,5-trimethoxy-1-[(3-acetamido-4-nitrophenyl)thio]benzene (ZLM-3)
[0084]
[0085] Add 3,4,5-trimethoxy-1-[(3-amino-4-nitrophenyl)thio]benzene ZLM-2 (50 mg) to a mixture of acetic anhydride (17 μL) and acetic acid (9 μL) In the solvent, reflux at 85-90°C for 2h. The low boiling point substances were evaporated under reduced pressure to obtain 61mg of yellow solid with a yield of 93%, mp168.1-170.2℃. 1 H NMR (400MHz, CDCl 3 ): δ2.26(s,3H),3.87(s,6H),3.92(s,3H),6.73(dd,J=7.2,1.8Hz,1H),6.81(s,2H),8.07(d, J=8.8Hz, 1H), 8.61(d, J=6.0Hz, 1H), 10.48(s, 1H). 13 CNMR (400MHz, CDCl3): δ25.7, 56.3, 61.0, 112.2, 117.6, 119.8, 123.7, 126.2, 132.9, 135.2, 139.6, 151.4, 154.0, 168.9. MS (EI) m / z: 378 (M + ).
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