反应 #4154638
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-08a0206c28b14e549af7006252c8237c暂无可渲染的结构数据
ClCC(NC1C=CC=CC=1C)=O产品信息
乙酰胺,2-氯-N-(2-甲基苯基)-(CAS 37394-93-7)的产品身份、结构标识及相关反应资料,供化学中间体检索、研发和采购评估使用。
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9 条反应 · 9 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-08a0206c28b14e549af7006252c8237c反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-7b69fd870c3848e5b726550ff5b677a7反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-08a0206c28b14e549af7006252c8237c反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-7b69fd870c3848e5b726550ff5b677a7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1-pyridin-2-ylpiperazine (24 mg, 0.15 mmol, Aldrich), N-(2-methyl-phenyl)-2-chloroacetamide (37 mg, 0.20 mmol, Maybridge) and sodium carbonate (50 mg) in N,N-dimethylformamide/water (2:1, 2 mL) was shaken at room temperature for 18 hours. The resulting mixture was decanted, concentrated under reduced pressure and the residue purified by preparative HPLC to provide 29.3 mg (63%) of the desired product. 1H NMR (500 MHz, DMSO-d6) δ 2.23 (s, 3H), 2.62 (t, J=4 Hz, 4H), 3.20 (s, 2H), 3.58 (t, J=4 Hz, 4H), 6.63 (t, J=5 Hz, 1H), 6.83 (d, J=6 Hz, 1H), 7.05 (t, J=6 Hz, 1H), 7.10 (m, 2H), 7.58 (t, J=5 Hz, 1H), 7.78 (d, J=6 Hz, 1H), 8.12 (d, J=5 Hz, 1H), 9.40 (s, 1H); MS (ESI/APCI+) m/e 311 (M+H)+. The resulting mixture was decanted concentrated under reduced pressure the residue purified by preparative HPLC
来源 ID: ord-d3fd871c2e7444a0ba4976baded35a99反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1-pyridin-2-ylpiperazine (24 mg, 0.15 mmol, Aldrich), N-(2-methyl-phenyl)-2-chloroacetamide (37 mg, 0.20 mmol, Maybridge) and sodium carbonate (50 mg) in N,N-dimethylformamide/water (2:1, 2 mL) was shaken at room temperature for 18 hours. The resulting mixture was decanted, concentrated under reduced pressure and the residue purified by preparative HPLC to provide 29.3 mg (63%) of the desired product. 1H NMR (500 MHz, DMSO-d6) δ 2.23 (s, 3H), 2.62 (t, J=4 Hz, 4H), 3.20 (s, 2H), 3.58 (t, J=4 Hz, 4H), 6.63 (t, J=5 Hz, 1H), 6.83 (d, J=6 Hz, 1H), 7.05 (t, J=6 Hz, 1H), 7.10 (m, 2H), 7.58 (t, J=5 Hz, 1H), 7.78 (d, J=6 Hz, 1H), 8.12 (d, J=5 Hz, 1H), 9.40 (s, 1H); MS (ESI/APCI+) m/e 311 (M+H)+. The resulting mixture was decanted concentrated under reduced pressure the residue purified by preparative HPLC
来源 ID: ord-d3fd871c2e7444a0ba4976baded35a99实验步骤: 投料: 将SM1(5g,27.2mmol,1.0eq),碳酸钾(11.3mmol,3.0eq),碘化钾(0.903g,5.44mmol,0.2eq),正丙胺(16g,272mmol,10eq)加入到封管中,乙腈(54ml)作溶剂,并升温至60℃搅拌6H. \n监测: 送样LCMS监测反应进程(19349-TM1-FD),未见原料,只有产物峰,停止反应。\n后处理: 将体系过滤,滤饼为盐,收集滤液加入水和EA萃取三次,合并有机相用饱和食盐水洗涤和无水硫酸钠干燥。\n纯化: 将粗品加入30mlEA稀释,滴加盐酸乙酸乙酯有大量白色固体析出,过滤,收集滤饼送样LCMS,HPLC(M-C4X-19349) 将产物冻干 2025.4.10 送样核磁和定量(M-C4X-19349/M-C4X-19349-Q) 2025.4.11 各项数据达标入库3.8438g白色固体。
来源 ID: 2206-M-C4X-19349-R1S1B1反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 3-azabicyclo[3.2.2]nonane (1.1 g) and triethylamine (0.88 g) in methylene chloride (25 ml) was added portionwise 2-chloroacetyl-6-methylaniline (1.47 g) under stirring and cooling in an ice-bath. After the addition was completed, the mixture was stirred at ambient temperature overnight. Removal of the solvent afforded a residue, which was dissolved in ethyl acetate and washed with water and brine. The organic layer was dried over magnesium sulfate and evaporated in vacuo to give a crystalline mass, which was pulverized in a mixture of n-hexane and diisopropyl ether. A dark yellow crystal was collected by filtration to give 2-[(3-azabicyclo[3.2.2]non-3-yl)acetyl]-6-methylaniline (1.92 g, 88.2%). cooling in an ice-bath After the addition the mixture was stirred at ambient temperature overnight Removal of the solvent afforded a residue, which washed with water and brine The organic layer was dried over magnesium sulfate evaporated in vacuo to give a crystalline mass, which A dark yellow crystal was collected by filtration
来源 ID: ord-d14438e7f5244894a3610c910765a481反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1-pyridin-2-ylpiperazine (24 mg, 0.15 mmol, Aldrich), N-(2-methyl-phenyl)-2-chloroacetamide (37 mg, 0.20 mmol, Maybridge) and sodium carbonate (50 mg) in N,N-dimethylformamide/water (2:1, 2 mL) was shaken at room temperature for 18 hours. The resulting mixture was decanted, concentrated under reduced pressure and the residue purified by preparative HPLC to provide 29.3 mg (63%) of the desired product. 1H NMR (500 MHz, DMSO-d6) δ 2.23 (s, 3H), 2.62 (t, J=4 Hz, 4H), 3.20 (s, 2H), 3.58 (t, J=4 Hz, 4H), 6.63 (t, J=5 Hz, 1H), 6.83 (d, J=6 Hz, 1H), 7.05 (t, J=6 Hz, 1H), 7.10 (m, 2H), 7.58 (t, J=5 Hz, 1H), 7.78 (d, J=6 Hz, 1H), 8.12 (d, J=5 Hz, 1H), 9.40 (s, 1H); MS (ESI/APCI+) m/e 311 (M+H)+. The resulting mixture was decanted concentrated under reduced pressure the residue purified by preparative HPLC
来源 ID: ord-d3fd871c2e7444a0ba4976baded35a99PubChem References
以下资料来自该化合物的公开数据库参考记录。
