反応 #4093603
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-42d0a2a304ff433c95ee028c94e43343表示可能な構造データがありません
CCOP(=O)(CCC1=CC=CC=C1)OCC製品情報
2-diethoxyphosphorylethylbenzene (CAS 54553-21-8) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 3448525
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-42d0a2a304ff433c95ee028c94e43343反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-b2d899b2ab83492585390d4db668c906反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature The DMF solution was distilled under reduced pressure leaving a residue The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-6cdc5fd140114cde9c4f1e2190f32365反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature The DMF solution was distilled under reduced pressure leaving a residue The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-6cdc5fd140114cde9c4f1e2190f32365反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In a manner according to Preparation 2 combine 2-phenylethyl bromide and triethyl phosphite. Distill the mixture at reduced pressure (0.15 mm Hg) and collect the fraction distilling at 115°-130° C. to obtain the title compound. Distill the mixture at reduced pressure (0.15 mm Hg) collect the fraction distilling at 115°-130° C.
ソース ID: ord-5fdc8f3c0f904a119539b199c5f50e6d反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. DMF was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature DMF was distilled off under reduced pressure the residue was dissolved in ethyl acetate The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-7c5f995c6a5f42f18e9fa1aeb49db21d反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature The DMF solution was distilled under reduced pressure leaving a residue The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-6cdc5fd140114cde9c4f1e2190f32365反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-42d0a2a304ff433c95ee028c94e43343反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature The DMF solution was distilled under reduced pressure leaving a residue The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-dcd0f02eba574f799999b6ccd76afd91反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature The DMF solution was distilled under reduced pressure leaving a residue The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-dcd0f02eba574f799999b6ccd76afd91反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In a manner according to Preparation 2 combine 2-phenylethyl bromide and triethyl phosphite. Distill the mixture at reduced pressure (0.15 mm Hg) and collect the fraction distilling at 115°-130° C. to obtain the title compound. Distill the mixture at reduced pressure (0.15 mm Hg) collect the fraction distilling at 115°-130° C.
ソース ID: ord-5fdc8f3c0f904a119539b199c5f50e6d反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. DMF was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5~137.5° C./3 mmHg. The mixture was stirred for 1 hour at not more than 0° C further the mixture was stirred overnight at room temperature DMF was distilled off under reduced pressure the residue was dissolved in ethyl acetate The ethyl acetate solution was washed with water dried with anhydrous sodium sulfate The solvent was evaporated the thus obtained oily product was distilled under reduced pressure
ソース ID: ord-7c5f995c6a5f42f18e9fa1aeb49db21dPubChem References
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