反应 #4121781
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-a998d78da043472e91d25b01154a079d暂无可渲染的结构数据
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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-a998d78da043472e91d25b01154a079d反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 2-tert-butyldimethylsilyloxy-4-nitroaniline (300 mg, 1.125 mmol) in toluene (10 mL), triphosgene (126 mg, 0.45 mmol) and triethylamine (0.195 mL, 1.35 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. Then it was cooled to room temperature and all solvent was evaporated. The residue was dissolved in DMF (1 mL) and 2-benzyloxypropylamine (185.6 mg, 1.125 mmol) was added. The reaction mixture was stirred at 80° C. for 16 hours. Chromatography of the resulting liquid on silica gel (50% Ethyl acetate/Hexane) gave desired product (160 mg, 41%). EI-MS m/z 346.4 (M+). mp: 64.6-65.2° C. Then it was cooled to room temperature all solvent was evaporated The residue was dissolved in DMF (1 mL) The reaction mixture was stirred at 80° C. for 16 hours
来源 ID: ord-07e213e56cea42cebb574def8e748fdd反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 2-tert-butyldimethylsilyloxy-4-nitroaniline (300 mg, 1.125 mmol) in toluene (10 mL), triphosgene (126 mg, 0.45 mmol) and triethylamine (0.195 mL, 1.35 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. Then it was cooled to room temperature and all solvent was evaporated. The residue was dissolved in DMF (1 mL) and 2-benzyloxypropylamine (185.6 mg, 1.125 mmol) was added. The reaction mixture was stirred at 80° C. for 16 hours. Chromatography of the resulting liquid on silica gel (50% Ethyl acetate/Hexane) gave desired product (160 mg, 41%). EI-MS m/z 346.4 (M+). mp: 64.6-65.2° C. Then it was cooled to room temperature all solvent was evaporated The residue was dissolved in DMF (1 mL) The reaction mixture was stirred at 80° C. for 16 hours
来源 ID: ord-07e213e56cea42cebb574def8e748fdd反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 2-tert-butyldimethylsilyloxy-4-nitroaniline (300 mg, 1.125 mmol) in toluene (10 mL), triphosgene (126 mg, 0.45 mmol) and triethylamine (0.195 mL, 1.35 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. Then it was cooled to room temperature and all solvent was evaporated. The residue was dissolved in DMF (1 mL) and 2-benzyloxypropylamine (185.6 mg, 1.125 mmol) was added. The reaction mixture was stirred at 80° C. for 16 hours. Chromatography of the resulting liquid on silica gel (50% Ethyl acetate/Hexane) gave desired product (160 mg, 41%). EI-MS m/z 346.4 (M+). mp: 64.6-65.2° C. Then it was cooled to room temperature all solvent was evaporated The residue was dissolved in DMF (1 mL) The reaction mixture was stirred at 80° C. for 16 hours
来源 ID: ord-07e213e56cea42cebb574def8e748fdd反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-a998d78da043472e91d25b01154a079d反应条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of styrene oxide (1.96 g, 0.010 mol) and 2-benzyloxypropylamine (2.48 g, 0.15 mol) was heated at 140° C. for 6 hours and then allowed to cool to ambient temperature and stand for 12 hours. The solidified reaction mixture was triturated with isooctane and filtered to obtain an impure solid that was recrystallized from isooctane to obtain 2.40 g of a white solid (84% yield); mp 90°-100° C. (undefined). to cool to ambient temperature The solidified reaction mixture was triturated with isooctane filtered to obtain an impure solid that was recrystallized from isooctane
来源 ID: ord-9930972b977f40ce97126d92214321de反应条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of trans-stilbene oxide (1.96 g, 0.010 mol) and 2-benzyloxypropylamine (2.48 g, 0.015 mol) was heated at 140° C. for 6 hours and then allowed to stand at ambient temperature for 12 hours. The solidified reaction mixture was triturated with petroleum ether and filtered to obtain 2.72 g of a solid. Mass spectral analysis showed starting materials present. Recrystallization from isooctane gave 2.16 g (60%) of the product as a white solid; mp 114°-119° C. The solidified reaction mixture was triturated with petroleum ether filtered
来源 ID: ord-439ae5a08b1241f3abeadb21b0bafc7d反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 2-tert-butyldimethylsilyloxy-4-nitroaniline (300 mg, 1.125 mmol) in toluene (10 mL), triphosgene (126 mg, 0.45 mmol) and triethylamine (0.195 mL, 1.35 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. Then it was cooled to room temperature and all solvent was evaporated. The residue was dissolved in DMF (1 mL) and 2-benzyloxypropylamine (185.6 mg, 1.125 mmol) was added. The reaction mixture was stirred at 80° C. for 16 hours. Chromatography of the resulting liquid on silica gel (50% Ethyl acetate/Hexane) gave desired product (160 mg, 41%). EI-MS m/z 346.4 (M+). mp: 64.6-65.2° C. Then it was cooled to room temperature all solvent was evaporated The residue was dissolved in DMF (1 mL) The reaction mixture was stirred at 80° C. for 16 hours
来源 ID: ord-07e213e56cea42cebb574def8e748fddPubChem References
以下资料来自该化合物的公开数据库参考记录。
