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C1CC(=O)CCCN(C1)CC2=CC=CC=C2製品情報
1-benzylazocan-5-one (CAS 16853-08-0) 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 59432979
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
9 反応 · 9 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-c1e452720062496989c795fa00e23d08反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (5 g, 14.9 mmol) over 5 hours in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hour. After being cooled, the reaction mixture was neuturalized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hour. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one. 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hour After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hour After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-da29af77a5bc4ea39610a10c464774eb反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (5 g, 14.9 mmol) over 5 hours in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hour. After being cooled, the reaction mixture was neuturalized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hour. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one. 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hour After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hour After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-67b5ca7d095d48f89f13d21369ceebb1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (5 g, 14.9 mmol) over 5 hours in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hour. After being cooled, the reaction mixture was neuturalized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hour. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one. 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hour After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hour After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-da29af77a5bc4ea39610a10c464774eb反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-c1e452720062496989c795fa00e23d08反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (O2) (5 g, 14.9 mmol) over 5 hrs in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hr. After being cooled, the reaction mixture was neutralized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hr. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one (O3). 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hr After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hr After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-cb72f34b616d469bbbb7a4cf9149af44反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (O2) (5 g, 14.9 mmol) over 5 hrs in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hr. After being cooled, the reaction mixture was neutralized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hr. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one (O3). 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hr After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hr After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-cb72f34b616d469bbbb7a4cf9149af44反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (5 g, 14.9 mmol) over 5 hours in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hour. After being cooled, the reaction mixture was neuturalized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hour. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one. 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hour After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hour After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-67b5ca7d095d48f89f13d21369ceebb1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred boiling slurry made from potassium (1.28 g, 32.8 mmol) and t-BuOH (2.43 g, 32.8 mmol) in xylene (182.5 mL) under N2 was added diethyl 4,4′-(benzylazanediyl)dibutanoate (5 g, 14.9 mmol) over 5 hours in xylene (37.25 mL). The mixture was stirred and heated at reflux for 1 hour. After being cooled, the reaction mixture was neuturalized with 6N HCl (100 mL) and then was extracted with 6N HCl (3×50 mL). The combined acid solutions were filtered and the filtrate was heated under reflux for 1 hour. After cooling, the mixture was basified with concentrated KOH solution to pH 10 with cooling and extracted with dichloromethane. The combined organics were dried over Na2SO4 and concentrated to give a residue. Another 17 batches were done in parallel. The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1) to give 1-benzylazocan-5-one. 1H NMR (CDCl3, 400 MHz) δ 7.30-7.33 (m, 2H), 7.21-7.25 (m, 3H), 3.56 (s, 2H), 2.55 (t, J=6.0, 4H), 2.24 (t, J=6.4 Hz, 4H), 1.86-1.91 (m, 4H). heated at reflux for 1 hour After being cooled was extracted with 6N HCl (3×50 mL) The combined acid solutions were filtered the filtrate was heated under reflux for 1 hour After cooling with cooling extracted with dichloromethane The combined organics were dried over Na2SO4 concentrated to give a residue The combined residue from 18 batches was purified together by column (P.E./EtOAc 5:1)
ソース ID: ord-da29af77a5bc4ea39610a10c464774ebPubChem References
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