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8 条反应 · 8 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-906825d989914d2297c9b0cad170934f反应条件: temp:70.01; pressure:0.00; stir:
实验步骤: Dilution of the aliquot (2 uL) with DMSO (200 uL).
来源 ID: ord-dd9ffc3f4ccf4e538b4f9d0cdfcf5b0a反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The title compound was prepared by a slightly modified literature procedure.* 3-aminophenyl methyl sulfone hydrochloride (1.18 g, 5.70 mmol) was suspended in water/CH2Cl2. The mixture was neutralized with 25% aqueous NaOH. The CH2Cl2 layer was isolated and evaporated to dryness. Aqueous H2SO4 (60%; 10 mL) was added to the residue and the solution was cooled to 0° C. A solution of NaNO2 (0.345 g, 5.00 mmol) in water (5 mL) was added dropwise. The solution was stirred at 0° C. for 30 min. and at 90° C. for 30 min. The reaction mixture was allowed to come to room temperature. Extraction with CH2Cl2, drying (MgSO4), and concentration gave 0.39 g (40%) of the title compound as a solid. MS m/z 172 (M)+. HRMS m/z calcd for C7H8O3S (M)+ 172.0194, found 172.0198. evaporated to dryness Aqueous H2SO4 (60%; 10 mL) was added to the residue to come to room temperature Extraction with CH2Cl2 drying (MgSO4), and concentration
来源 ID: ord-b14b87f5bb384528ab0bafa84a3ffdc1反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The title compound was prepared by a slightly modified literature procedure.* 3-aminophenyl methyl sulfone hydrochloride (1.18 g, 5.70 mmol) was suspended in water/CH2Cl2. The mixture was neutralized with 25% aqueous NaOH. The CH2Cl2 layer was isolated and evaporated to dryness. Aqueous H2SO4 (60%; 10 mL) was added to the residue and the solution was cooled to 0° C. A solution of NaNO2 (0.345 g, 5.00 mmol) in water (5 mL) was added dropwise. The solution was stirred at 0° C. for 30 min. and at 90° C. for 30 min. The reaction mixture was allowed to come to room temperature. Extraction with CH2Cl2, drying (MgSO4), and concentration gave 0.39 g (40%) of the title compound as a solid. MS m/z 172 (M)+. HRMS m/z calcd for C7H8O3S (M)+ 172.0194, found 172.0198. evaporated to dryness Aqueous H2SO4 (60%; 10 mL) was added to the residue to come to room temperature Extraction with CH2Cl2 drying (MgSO4), and concentration
来源 ID: ord-b14b87f5bb384528ab0bafa84a3ffdc1反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-906825d989914d2297c9b0cad170934f反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1-Methoxy-3-(methylsulfonyl)benzene (300 mg, 1.61 mmol) was suspended in 1.6 mL aqueous hydrobromic acid (48% w/w) and 1.6 mL acetic acid. The mixture was heated under reflux for 24 hours. The reaction was cooled back to room temperature and concentrated. The residue was purified by column chromatography through a 40 gram biotage silica gel cartridge eluting with 40-70% ethyl acetate/hexanes (gradient) to give the product as white solid. LRMS calc: 172.0; obs: 173.2 (M+1). The mixture was heated under reflux for 24 hours concentrated The residue was purified by column chromatography through a 40 gram biotage silica gel cartridge eluting with 40-70% ethyl acetate/hexanes (gradient)
来源 ID: ord-11b48ec471dc4eb293cd2916ea000e55反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The title compound was prepared by a slightly modified literature procedure.*3-aminophenyl methyl sulfone hydrochloride (1.18 g, 5.70 mmol) was suspended in water/CH2Cl2. The mixture was neutralized with 25% aqueous NaOH. The CH2Cl2 layer was isolated and evaporated to dryness. Aqueous H2SO4 (60%; 10 mL) was added to the residue and the solution was cooled to 0° C. A solution of NaNO2 (0.345 g, 5.00 mmol) in water (5 mL) was added dropwise. The solution was stirred at 0° C. for 30 min. and at 90° C. for 30 min. The reaction mixture was allowed to come to room temperature. Extraction with CH2Cl2, drying (MgSO4), and concentration gave 0.39 g (40%) of the title compound as a solid. MS m/z 172 (M)+. HRMS m/z calcd for C7H8O3S (M)+172.0194, found 172.0198. The title compound was prepared by a slightly modified literature procedure evaporated to dryness Aqueous H2SO4 (60%; 10 mL) was added to the residue to come to room temperature Extraction with CH2Cl2 drying (MgSO4), and concentration
来源 ID: ord-45c3ff1bfa84413d9285baf79542ac92反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The title compound was prepared by a slightly modified literature procedure.* 3-aminophenyl methyl sulfone hydrochloride (1.18 g, 5.70 mmol) was suspended in water/CH2Cl2. The mixture was neutralized with 25% aqueous NaOH. The CH2Cl2 layer was isolated and evaporated to dryness. Aqueous H2SO4 (60%; 10 mL) was added to the residue and the solution was cooled to 0° C. A solution of NaNO2 (0.345 g, 5.00 mmol) in water (5 mL) was added dropwise. The solution was stirred at 0° C. for 30 min. and at 90° C. for 30 min. The reaction mixture was allowed to come to room temperature. Extraction with CH2Cl2, drying (MgSO4), and concentration gave 0.39 g (40%) of the title compound as a solid. MS m/z 172 (M)+. HRMS m/z calcd for C7H8O3S (M)+ 172.0194, found 172.0198. evaporated to dryness Aqueous H2SO4 (60%; 10 mL) was added to the residue to come to room temperature Extraction with CH2Cl2 drying (MgSO4), and concentration
来源 ID: ord-b14b87f5bb384528ab0bafa84a3ffdc1PubChem References
以下资料来自该化合物的公开数据库参考记录。