反応 #4050603
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-00a90e7928e04e4bb187c8cfd882046a表示可能な構造データがありません
IC1C=CC(=C(C=1)N)F製品情報
2-FLUORO-5-IODO-PHENYLAMINE (CAS 886362-82-9) 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 25418460
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
7 反応 · 7 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-00a90e7928e04e4bb187c8cfd882046a反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-00a90e7928e04e4bb187c8cfd882046a反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs). was added the above solution at 0° C The precipitates were collected by filtration washed with water dissolved in EtOAc washed with brine dried over MgSO4 filtered concentrated in vacuo
ソース ID: ord-cd174c10c5cb45aa86438f61c82f1e5a反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs). was added the above solution at 0° C The precipitates were collected by filtration washed with water dissolved in EtOAc washed with brine dried over MgSO4 filtered concentrated in vacuo
ソース ID: ord-04543525e77c43b7b8a892ddd0fe211d反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs). was added the above solution at 0° C The precipitates were collected by filtration washed with water dissolved in EtOAc washed with brine dried over MgSO4 filtered concentrated in vacuo
ソース ID: ord-44a57e8c78144373930310eda9d9e1d3反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs). was added the above solution at 0° C The precipitates were collected by filtration washed with water dissolved in EtOAc washed with brine dried over MgSO4 filtered concentrated in vacuo
ソース ID: ord-6142beb941634b0a97b92eec75fc9b5f反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs). was added the above solution at 0° C The precipitates were collected by filtration washed with water dissolved in EtOAc washed with brine dried over MgSO4 filtered concentrated in vacuo
ソース ID: ord-8b785afee0534bcba6b55d644533611fPubChem References
化合物の公開データベース記録に掲載された情報源です。
