反応 #4120882
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-c86ce5a76b1445bbb825cf421671bfd6表示可能な構造データがありません
ClC(C(F)(F)F)=NC1C=CC=CC=1製品情報
2,2,2-Trifluoro-N-phenylacetimidoyl Chloride (CAS 61881-19-4) 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 10058869
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-c86ce5a76b1445bbb825cf421671bfd6反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-d0b750179e254cb388baeaa26f336e2b反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-4b309c03d2924cf3a3b1809b4b5819f5反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of Ph3P (138.0 g, 526 mmol), Et3N (21.3 g, 211 mmol), CCl4 (170 mL) and TFA (20 g, 175 mmol) was stirred for 10 min in an ice-bath. Aniline (19.6 g, 211 mmol) was dissolved in CCl4 (20 mL) was added. The mixture was stirred at reflux for 3 h. The solvent was removed under vacuum and hexane was added. The precipitates (Ph3PO and Ph3P) were filtered off and washed with hexane. The filtrate was distilled under reduced pressure to yield 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g), which was used in the next step without further purification. was added The mixture was stirred at reflux for 3 h The solvent was removed under vacuum and hexane was added The precipitates (Ph3PO and Ph3P) were filtered off washed with hexane The filtrate was distilled under reduced pressure
ソース ID: ord-bec768f200cc4feb9b1402275930c404反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-3ca47f9df6174b51b7bc3ad10325c767反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of Ph3P (138.0 g, 526 mmol), Et3N (21.3 g, 211 mmol), CCl4 (170 mL) and TFA (20 g, 175 mmol) was stirred for 10 min in an ice-bath. Aniline (19.6 g, 211 mmol) was dissolved in CCl4 (20 mL) was added. The mixture was stirred at reflux for 3 h. The solvent was removed under vacuum and hexane was added. The precipitates (Ph3PO and Ph3P) were filtered off and washed with hexane. The filtrate was distilled under reduced pressure to yield 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g), which was used in the next step without further purification. was added The mixture was stirred at reflux for 3 h The solvent was removed under vacuum and hexane was added The precipitates (Ph3PO and Ph3P) were filtered off washed with hexane The filtrate was distilled under reduced pressure
ソース ID: ord-e07c29ab4005418ea75ae36d4e7a85f3反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-251656782daf429db4f0c882a5d92e3e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-251656782daf429db4f0c882a5d92e3e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of Ph3P (138.0 g, 526 mmol), Et3N (21.3 g, 211 mmol), CCl4 (170 mL) and TFA (20 g, 175 mmol) was stirred for 10 min in an ice-bath. Aniline (19.6 g, 211 mmol) was dissolved in CCl4 (20 mL) was added. The mixture was stirred at reflux for 3 h. The solvent was removed under vacuum and hexane was added. The precipitates (Ph3PO and Ph3P) were filtered off and washed with hexane. The filtrate was distilled under reduced pressure to yield 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g), which was used in the next step without further purification. was added The mixture was stirred at reflux for 3 h The solvent was removed under vacuum and hexane was added The precipitates (Ph3PO and Ph3P) were filtered off washed with hexane The filtrate was distilled under reduced pressure
ソース ID: ord-ebc842e3e0e445aca877b7094142c522反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-4b309c03d2924cf3a3b1809b4b5819f5反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of Ph3P (138.0 g, 526 mmol), Et3N (21.3 g, 211 mmol), CCl4 (170 mL) and TFA (20 g, 175 mmol) was stirred for 10 min in an ice-bath. Aniline (19.6 g, 211 mmol) was dissolved in CCl4 (20 mL) was added. The mixture was stirred at reflux for 3 h. The solvent was removed under vacuum and hexane was added. The precipitates (Ph3PO and Ph3P) were filtered off and washed with hexane. The filtrate was distilled under reduced pressure to yield 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g), which was used in the next step without further purification. was added The mixture was stirred at reflux for 3 h The solvent was removed under vacuum and hexane was added The precipitates (Ph3PO and Ph3P) were filtered off washed with hexane The filtrate was distilled under reduced pressure
ソース ID: ord-bec768f200cc4feb9b1402275930c404反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of NaH (3.47 g, 145 mmol, 60% in mineral oil) in THF (200 mL) was added diethyl malonate (18.5 g, 116 mmol) at 0° C. The mixture was stirred for 30 min at this temperature and 2,2,2-trifluoro-N-phenyl-acetimidoyl chloride (19 g, 92 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The mixture was diluted with CH2Cl2, washed with saturated sodium bicarbonate solution and brine. The combined organic layers were dried over Na2SO4, filtered and concentrated to provide 2-(2,2,2-trifluoro-1-phenylimino-ethyl)-malonic acid diethyl ester, which was used directly in the next step without further purification. was added at 0° C washed with saturated sodium bicarbonate solution and brine The combined organic layers were dried over Na2SO4 filtered concentrated
ソース ID: ord-3ca47f9df6174b51b7bc3ad10325c767PubChem References
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