Substituted thienobenzoquinone compounds and their preparation methods and applications
A compound and synthesis method technology, applied in the field of medicine, can solve the problems of lack of antifungal drugs, low bioavailability, limited clinical application, etc., and achieve the effect of broad-spectrum antifungal activity
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Embodiment 1
[0050] Example 1: Preparation of 5-azido-2-nitrobenzo[b]thiophene-4,7-dione (1)
[0051] Take 5-bromo-2-nitrobenzo[b]thiophene-4,7-dione (1.43g, 5mmol) and dissolve it in 15mL of methanol, dichloromethane and water mixture (volume ratio is 9:2: 2) Then add solid sodium azide (812mg, 2.5eq) and continue to stir at room temperature for 2 hours. Dichloromethane was added to the reaction solution for extraction, the aqueous phase was adjusted to pH=11 with 10% sodium hydroxide solution, and then NaClO solution was added to quench the excess sodium azide. After the organic phase was dried, it was spin-dried to obtain a brown solid powder (1.13g, yield: 90.2%). 1 HNMR(400MHz, CDCl 3 )δppm: 8.25 (s, 1H), 6.46 (s, 1H).
Embodiment 2
[0052] Example 2: Preparation of 5-methoxy-2-nitrobenzo[b]thiophen-4,7-dione (2)
[0053] Add the raw material 5-bromo-2-nitrobenzo[b]thiophen-4,7-dione (27.4mg, 0.1mmol) to the mixed solvent of toluene (5mL) and methanol (0.5mL), and then add cesium carbonate solid (47mg, 0.14mmol, 1.50eq), stirred at room temperature for 1 hour. The reaction solution was extracted with ethyl acetate, dried, and the solvent was removed. The residue was separated on a silica gel column (developing solvent: 70% petroleum ether 30% ethyl acetate) to obtain 17.8 mg of a yellow solid with a yield of 77.3%. 1 H NMR(400MHz, CDCl 3 )δppm: 3.95 (s, 3H) 6.18 (s, 1H) 8.28 (s, 1H).
[0054] Compound 3 can be obtained by repeating the steps in Example 2.
Embodiment 3
[0055] Example 3: Preparation of 5-azido-benzo[b]thiophene-4,7-dione (Ⅲ)
[0056] Take 5-bromo-benzo[b]thiophene-4,7-dione (1.21g, 5mmol) and dissolve it in a mixture of 20mL methanol, dichloromethane and water (volume ratio 9:2:2), then Add solid sodium azide (812 mg, 2.5 eq) and continue stirring at room temperature for 2 hours. Dichloromethane was added to the reaction solution for extraction, the aqueous phase was adjusted to pH=11 with 10% sodium hydroxide solution, and then NaClO solution was added to quench the excess sodium azide. After the organic phase is dried, it is spin-dried to obtain a brown solid powder (0.91g, yield: 88.8%). 1 H NMR(400MHz, CDCl 3 )δppm: 7.67(d,J=4.8Hz,1H), 7.58(d,J=4.8Hz,1H), 6.34(s,1H).
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