Benzo [c] [1, 2] oxaborolane-1 (3H)-alcohol compound and application thereof
A compound and hydrate technology, applied in the field of biomedicine, can solve problems such as central nervous system disorders, and achieve high activity, good regulatory activity, and good economic value.
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Embodiment 1
[0048] 2-((1-Hydroxy-1,3-dihydrobenzo[c][1,2]oxaborin-6-yl)methyl)-1-oxo-1,2,3,4 -Tetrahydroisoquinoline-6-carbonitrile
[0049]
[0050] first step:
[0051] Compound 1a (31.4g, 200.0mmol) and methanesulfonic acid (50ml) were dissolved in dichloromethane (200ml), and NaN was added under ice-cooling 3 (26g, 400.0mmol), stirred and reacted at room temperature for 12 hours, TLC detected the reaction, after the reaction was completed, the reaction solution was poured into 10% aqueous sodium hydroxide solution (500ml), extracted with dichloromethane (200ml×2), the combined organic layers were dried, Column chromatography separated to obtain 25.7 g of off-white solid with a yield of 74.7%.
[0052] Step two:
[0053] Compound 1b (25.0g, 145.3mmol) was dissolved in DMF (200ml), sodium hydride (4.2g, 174.4mmol) was added at room temperature, stirred for 1 hour, then compound 1c (44.4g, 145.3mmol) was added, at 40°C The reaction was stirred for 4 hours, and the reaction was det...
Embodiment 2
[0059] 2-((1-Hydroxy-1,3-dihydrobenzo[c][1,2]oxaborin-6-yl)methyl)-1-oxo-1,2,3,4 -Tetrahydroisoquinoline-5-carbonitrile
[0060]
[0061] first step:
[0062] Compound 2a (15.7g, 100.0mmol) and methanesulfonic acid (30ml) were dissolved in dichloromethane (200ml), and NaN3 (13g, 200.0mmol) was added under ice-cooling, stirred at room temperature for 12 hours, and TLC detected the reaction. After the reaction was completed, the reaction solution was poured into 10% aqueous sodium hydroxide solution (500ml), extracted with dichloromethane (200ml×2), the organic layers were combined, dried, and separated by column chromatography to obtain 12.1g of an off-white solid with a yield of 70.3%.
[0063] Step two:
[0064] Compound 2b (12.0g, 69.8mmol) was dissolved in DMF (100ml), sodium hydride (3.3g, 137.5mmol) was added at room temperature, stirred for 1 hour, then compound 1c (21.4g, 69.8mmol) was added, at 40°C The reaction was stirred for 4 hours, and the reaction was detec...
Embodiment 3
[0070] 2-((1-Hydroxy-1,3-dihydrobenzo[c][1,2]oxaborin-6-yl)methyl)-1-oxo-1,2,3,4 -Tetrahydroisoquinoline-7-carbonitrile
[0071]
[0072] first step:
[0073] Compound 3a (15.7g, 100.0mmol) and methanesulfonic acid (30ml) were dissolved in dichloromethane (200ml), and NaN was added under ice-cooling 3 (13.0g, 200.0mmol), stirred and reacted at room temperature for 12 hours, TLC detected the reaction, after the reaction was completed, the reaction solution was poured into 10% aqueous sodium hydroxide solution (500ml), extracted with dichloromethane (200ml×2), the organic layers were combined, and dried , and separated by column chromatography to obtain 12.7 g of off-white solid with a yield of 73.8%.
[0074] The second step to the fourth step refer to Example 1 to obtain the title compound (off-white solid 1.5 g, yield 47.2%), ESI (+) m / z = 319.1.
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