反応 #4047410
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-3c27be6161d14fe1b0e08f9a2b238f6e表示可能な構造データがありません
C1=CC(=C(C=C1Cl)C(=O)N)F製品情報
5-chloro-2-fluorobenzamide (CAS 261762-57-6) 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 2773592
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-3c27be6161d14fe1b0e08f9a2b238f6e反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-73727865c88f48439b09bca5cfee3706反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A method similar to the preparation of 5-chloro-2-fluorobenzamide (see page 17 above) was followed using 4-chloro-2-fluorobenzoic acid (500 mg, 5.73 mmol). The title compound was isolated as an off-white solid (465 mg, 94%).
ソース ID: ord-4b299c36ce824333845cec6832f142c4反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A method similar to the preparation of 5-chloro-2-fluorobenzamide (see page 17 above) was followed using 4-chloro-2-fluorobenzoic acid (500 mg, 5.73 mmol). The title compound was isolated as an off-white solid (465 mg, 94%).
ソース ID: ord-4b299c36ce824333845cec6832f142c4反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Benzyl mercaptan (0.61 mL, 5.20 mmol) was added dropwise over 10 min to a stirred suspension of sodium hydride (60% in oil, 230 mg, 5.75 mmol) in THF (10 mL) at ambient temperature under a nitrogen atmosphere. The white suspension was stirred for a further 1 h and then added dropwise to a stirred solution of 5-chloro-2-fluorobenzamide (900 mg, 5.20 mmol) in THF (10 mL), under nitrogen, over 10 min. The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h and at reflux for 3 h and then quenched with water (200 mL). The product mixture was extracted with EtOAc (3×30 mL) and the combined extracts washed with brine (50 mL), dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2, v/v) as eluent to give the title compound as a white solid (523 mg, 36%). The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h at reflux for 3 h quenched with water (200 mL) The product mixture was extracted with EtOAc (3×30 mL) the combined extracts washed with brine (50 mL) dried (MgSO4) concentrated in vacuo The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2
ソース ID: ord-6cbe3f07c3e24df78ac0e1d912c00f34反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Benzyl mercaptan (0.61 mL, 5.20 mmol) was added dropwise over 10 min to a stirred suspension of sodium hydride (60% in oil, 230 mg, 5.75 mmol) in THF (10 mL) at ambient temperature under a nitrogen atmosphere. The white suspension was stirred for a further 1 h and then added dropwise to a stirred solution of 5-chloro-2-fluorobenzamide (900 mg, 5.20 mmol) in THF (10 mL), under nitrogen, over 10 min. The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h and at reflux for 3 h and then quenched with water (200 mL). The product mixture was extracted with EtOAc (3×30 mL) and the combined extracts washed with brine (50 mL), dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2, v/v) as eluent to give the title compound as a white solid (523 mg, 36%). The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h at reflux for 3 h quenched with water (200 mL) The product mixture was extracted with EtOAc (3×30 mL) the combined extracts washed with brine (50 mL) dried (MgSO4) concentrated in vacuo The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2
ソース ID: ord-6cbe3f07c3e24df78ac0e1d912c00f34反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A method similar to the preparation of 5-chloro-2-fluorobenzamide (see page 17 above) was followed using 4-chloro-2-fluorobenzoic acid (500 mg, 5.73 mmol). The title compound was isolated as an off-white solid (465 mg, 94%).
ソース ID: ord-4b299c36ce824333845cec6832f142c4反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Benzyl mercaptan (0.61 mL, 5.20 mmol) was added dropwise over 10 min to a stirred suspension of sodium hydride (60% in oil, 230 mg, 5.75 mmol) in THF (10 mL) at ambient temperature under a nitrogen atmosphere. The white suspension was stirred for a further 1 h and then added dropwise to a stirred solution of 5-chloro-2-fluorobenzamide (900 mg, 5.20 mmol) in THF (10 mL), under nitrogen, over 10 min. The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h and at reflux for 3 h and then quenched with water (200 mL). The product mixture was extracted with EtOAc (3×30 mL) and the combined extracts washed with brine (50 mL), dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2, v/v) as eluent to give the title compound as a white solid (523 mg, 36%). The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h at reflux for 3 h quenched with water (200 mL) The product mixture was extracted with EtOAc (3×30 mL) the combined extracts washed with brine (50 mL) dried (MgSO4) concentrated in vacuo The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2
ソース ID: ord-6cbe3f07c3e24df78ac0e1d912c00f34反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-3c27be6161d14fe1b0e08f9a2b238f6e反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-73727865c88f48439b09bca5cfee3706反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A method similar to the preparation of 5-chloro-2-fluorobenzamide (see page 17 above) was followed using 4-chloro-2-fluorobenzoic acid (500 mg, 5.73 mmol). The title compound was isolated as an off-white solid (465 mg, 94%).
ソース ID: ord-4b299c36ce824333845cec6832f142c4反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Benzyl mercaptan (0.61 mL, 5.20 mmol) was added dropwise over 10 min to a stirred suspension of sodium hydride (60% in oil, 230 mg, 5.75 mmol) in THF (10 mL) at ambient temperature under a nitrogen atmosphere. The white suspension was stirred for a further 1 h and then added dropwise to a stirred solution of 5-chloro-2-fluorobenzamide (900 mg, 5.20 mmol) in THF (10 mL), under nitrogen, over 10 min. The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h and at reflux for 3 h and then quenched with water (200 mL). The product mixture was extracted with EtOAc (3×30 mL) and the combined extracts washed with brine (50 mL), dried (MgSO4) and concentrated in vacuo. The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2, v/v) as eluent to give the title compound as a white solid (523 mg, 36%). The mixture was stirred at ambient temperature for 1 h, at 50° C. for 1 h at reflux for 3 h quenched with water (200 mL) The product mixture was extracted with EtOAc (3×30 mL) the combined extracts washed with brine (50 mL) dried (MgSO4) concentrated in vacuo The crude product was purified by chromatography on silica gel with EtOAc:heptane (3:2
ソース ID: ord-6cbe3f07c3e24df78ac0e1d912c00f34PubChem References
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