Indole derivative and preparation method thereof
A compound, hydrate technology, applied in the field of new antibacterial compounds, can solve problems such as no obvious antibacterial effect
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Embodiment 1
[0328] Example 1: 2-Carboxylic acid-3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole (compound C)
[0329]
[0330] Step 1) Under nitrogen protection, slowly add tin tetrachloride (4.5ml, 36mmol) to a solution of 4-iodoindole (7.5g, 30mmol) in dichloromethane (75ml) at 0°C, react at room temperature for 30min, and then Join Ac 2 O (2.9g, 30mmol) and nitromethane (46.5ml), reacted at room temperature for 1h, quenched with ice water, filtered, the filter cake was washed with a small amount of ether, the organic layer was extracted with ethyl acetate, anhydrous Na 2 SO 4 After drying, the solvent was spin-dried and recrystallized with ethyl acetate and petroleum ether to obtain compound 3-acetyl-4-iodoindole (6.9 g, 78%).
[0331] 1 HNMR(500MHz,DMSO-d6)δ:12.07(s,1H),8.32(d,J=3.0Hz,1H),7.67(dd,J=7.5Hz,1.0Hz,1H),7.49(dd,J= 8.0Hz, 1.0Hz, 1H), 6.92(t, J=8.0Hz, 1H), 2.49(s, 3H). MS (ESI + )m / z:286.0[M+H] + .
[0332] Step 2) Under nitrogen protection, mix 3-acetyl-4-iodoi...
Embodiment 2
[0341] Example 2: Benzoyloxymethyl 3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole-2-carboxylate (CV2)
[0342]
[0343] Under nitrogen protection, the racemic mixture 2-carboxylic acid-3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole or (2R,3S)-2 -Carboxylic acid-3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole (0.23g, 1mmol) and triethylamine (0.10g, 1mmol) dissolved In DMF solution (6ml), react at room temperature for 5min, then add chloromethyl benzoate (0.17g, 1mmol), react at room temperature for 24h, add ethyl acetate 50ml after the reaction, wash the ethyl acetate layer (80ml×3 ), the ethyl acetate layer was washed with anhydrous Na 2 SO 4 After drying, the solvent was spin-dried and recrystallized with ethanol and petroleum ether to obtain a racemic mixture of 3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole-2-carboxylate Benzoyloxymethyl ester or (2R,3S)-3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole-2-carboxylic acid benzene Formyloxymethyl ester...
Embodiment 3
[0345] Example 3: 3-(Indol-3-yl)-butyric acid (Compound 20)
[0346]
[0347] Sodium hydroxide (0.19g, 4.8mmol) was dissolved in water (50ml), and the racemic mixture 2-carboxylic acid-3-methyl-3,5-dihydro-2H-thiopyrano[ 4,3,2-cd]indole or (2R,3S)-2-carboxylic acid-3-methyl-3,5-dihydro-2H-thiopyrano[4,3,2-cd]indole Indole (1g, 4.3mmol), add freshly prepared Raney nickel (Raney nickel) (10g, wet weight, containing absolute ethanol) and water (50ml) to it, heat and reflux for 1 hour, cool and filter, and use 0.02% Wash with sodium hydroxide solution (20ml×2), combine the washing solution with the filtrate, add 0.2 g of activated carbon for decolorization, filter, acidify the filtrate with concentrated hydrochloric acid and extract with ether (20ml×3), wash the ether extract with water (10ml×3) , dried over night over anhydrous sodium sulfate, concentrated solvent and recrystallized with diethyl ether and petroleum ether to obtain yellow crystals, which is a racemic mixture of ...
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