Preparation method of 7-alkylindole derivative
A technology of alkyl indole derivatives and indole, applied in the production of bulk chemicals, organic chemistry, etc., to achieve the effects of mild conditions, environmental friendliness, and low cost
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Embodiment 1
[0029] Preparation of 7-methyl-1H-indole
[0030] In a 50 mL stainless steel grinding jar add N -Pyrimidine indole (97.5 mg, 0.5 mmol), methyl bromide (235.0 mg, 2.5 mmol), Mn(OAc) 2 (17.3 mg, 0.1 mmol), magnesium granules (10-30 mesh) (72.9 mg, 3.0 mmol), N 1 , N 1 ,N 2 , N 2 -Tetraethylethane-1,2-diamine (172.5 mg, 1.0 mmol), and then add 1 stainless steel ball with a diameter of 14 mm, tighten the grinding jar, put it into a vibrating grinder, and grind it at 30 Hz Grind at frequency for 90 minutes. After the reaction was completed, the entire reaction mixture was poured out from the grinding jar, and the stainless steel ball was taken out, quenched with 10 mL of saturated ammonium chloride solution, extracted with ethyl acetate (3×10 mL), and the organic layers were combined and concentrated under reduced pressure. Then use petroleum ether and ethyl acetate (volume ratio 20:1) as the eluent for column chromatography separation, the obtained eluent is evaporated to re...
Embodiment 2
[0032] Preparation of 7-ethyl-1H-indole
[0033] Add to 80 mL stainless steel grinding jar N -Pyrimidine indole (97.5 mg, 0.5 mmol), bromoethane (54.5 mg, 0.5 mmol), Mn(acac) 3 (88.1 mg, 0.25 mmol), magnesium granules (10-30 mesh) (12.2 mg, 0.5 mmol), N 1 ,N 1 , N 2 , N 2 -Tetraethylethane-1,2-diamine (431.3 mg, 2.5 mmol), then add 20 stainless steel balls with a diameter of 8 mm, tighten the grinding jar, put it into a planetary grinder, and set it at a frequency of 800 rpm Grind down for 60 minutes. After the reaction was completed, the entire reaction mixture was poured out from the grinding jar, and the stainless steel ball was taken out, quenched with 10 mL of saturated ammonium chloride solution, extracted with ethyl acetate (3×10 mL), and the organic layers were combined and concentrated under reduced pressure. Then use petroleum ether and ethyl acetate (volume ratio 20:1) as the eluent for column chromatography separation, the obtained eluent is evaporated to rem...
Embodiment 3
[0035] Preparation of 7-isopropyl-1H-indole
[0036] In a 15 mL stainless steel grinding jar add N -Pyrimidine indole (97.5 mg, 0.5 mmol), 2-bromopropane (369.0 mg, 3.0 mmol), MnCl 2 (31.5 mg, 0.25 mmol), magnesium foil (0.1~0.5 mm thick) (60.7 mg, 2.5 mmol), 1,3-methyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (320.4 mg, 2.5 mmol), and then add 2 stainless steel balls with a diameter of 6 mm, tighten the grinding jar, put it into a vibrating grinder, and grind at a frequency of 10 Hz for 120 minutes. After the reaction was completed, the entire reaction mixture was poured out from the grinding jar, and the stainless steel ball was taken out, quenched with 10 mL of saturated ammonium chloride solution, extracted with ethyl acetate (3×10 mL), and the organic layers were combined and concentrated under reduced pressure. Then use petroleum ether and ethyl acetate (volume ratio 20:1) as the eluent for column chromatography separation, the obtained eluent is evaporated to remove the ...
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