反应 #4149685
相关文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0112905da16f4581826db13c9e958617暂无可渲染的结构数据
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12 条反应 · 12 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0112905da16f4581826db13c9e958617反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-ef6679938b5c438391d5f93f7de26a58反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-0112905da16f4581826db13c9e958617反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with cone. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. Then the reaction mixture was slowly treated with cone poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-74a5fb5bb01245bbb47f1e85f9104d48反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with cone. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. Then the reaction mixture was slowly treated with cone poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-74a5fb5bb01245bbb47f1e85f9104d48反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-ef6679938b5c438391d5f93f7de26a58反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with cone. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. Then the reaction mixture was slowly treated with cone poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-74a5fb5bb01245bbb47f1e85f9104d48反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ−128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-8fd18f2a2cbb42c5bea2bed7b62789a3反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ−128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-8fd18f2a2cbb42c5bea2bed7b62789a3反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-3985cf0dd6374b52bd2217be380eeca9反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-3985cf0dd6374b52bd2217be380eeca9反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05. while maintaining the internal temperature below 20° C poured onto ice (300 g) the oily layer was extracted with CH2Cl2 (2×125 ml) The organic layer was washed with water (2×200 ml), brine (200 ml) dried (MgSO4) evaporated to obtain the crude product which was purified over flash silica gel chromatography
来源 ID: ord-855fb0cdcc5b4f2fb2ccbec040925199PubChem References
以下资料来自该化合物的公开数据库参考记录。
