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CC1=C(C=CC(=C1)Br)OC(F)F製品情報
4-Bromo-1-(difluoromethoxy)-2-methylbenzene (CAS 888327-32-0) 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 45158710
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-ae778e093b224a81a3fc42448309eaed反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-3610792d2a8b4de2b3bd76d8e2bd3784反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-8f133474bd3b4b51ad5da2956d77a7b9反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-ae778e093b224a81a3fc42448309eaed反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-3610792d2a8b4de2b3bd76d8e2bd3784反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To 4-bromo-1-(difluoromethoxy)-2-methylbenzene (2.36 g, 10.00 mmol) in toluene (50 mL) was added cis-2,6-dimethylpiperazine (5 g, 58.14 mmol), Pd(OAc)2 (120 mg, 0.53 mmol), BINAP (380 mg, 0.61 mmol), and t-BuOK (2.2 g, 19.64 mmol). The resulting solution was stirred for 4 hours at 80° C. The solution was cooled to room temperature and washed with H2O (2×50 mL), dried over Na2SO4, concentrated, and purified by silica gel column chromatography (10:1 CH2Cl2/MeOH) to give 1.1 g (41%) of 1-(4-(difluoromethoxy)-3-methylphenyl)-3,5-dimethylpiperazine. The solution was cooled to room temperature washed with H2O (2×50 mL) dried over Na2SO4 concentrated purified by silica gel column chromatography (10:1 CH2Cl2/MeOH)
ソース ID: ord-b2ae8fadf11640e3a132f402d609ade1反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred solution of 4-amino-1-difluoromethoxy-2-methyl-benzene (5 g, 28.90 mmol) in HBr (20 mL) and water (20 mL) at 0° C. was added a solution of sodium nitrite (2.07 g, 30.00 mmol) in H2O (10 ml) dropwise over a period of 20 minutes. After the addition was complete, the reaction mixture was stirred for 30 minutes at 0° C. Copper (I) bromide (4 g, 27.87 mmol) was then added and the mixture was heated at 60° C. for 30 minutes. The resulting solution was extracted with EtOAc (3×50 mL) and the combined organic layers washed with H2O (1×20 mL), dried over Na2SO4 and concentrated to provide 2.5 g (37%) of 4-bromo-1-(difluoromethoxy)-2-methylbenzene. After the addition the mixture was heated at 60° C. for 30 minutes The resulting solution was extracted with EtOAc (3×50 mL) the combined organic layers washed with H2O (1×20 mL) dried over Na2SO4 concentrated
ソース ID: ord-64474ff9992e45518168107afa9f587c反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred solution of 4-amino-1-difluoromethoxy-2-methyl-benzene (5 g, 28.90 mmol) in HBr (20 mL) and water (20 mL) at 0° C. was added a solution of sodium nitrite (2.07 g, 30.00 mmol) in H2O (10 ml) dropwise over a period of 20 minutes. After the addition was complete, the reaction mixture was stirred for 30 minutes at 0° C. Copper (I) bromide (4 g, 27.87 mmol) was then added and the mixture was heated at 60° C. for 30 minutes. The resulting solution was extracted with EtOAc (3×50 mL) and the combined organic layers washed with H2O (1×20 mL), dried over Na2SO4 and concentrated to provide 2.5 g (37%) of 4-bromo-1-(difluoromethoxy)-2-methylbenzene. After the addition the mixture was heated at 60° C. for 30 minutes The resulting solution was extracted with EtOAc (3×50 mL) the combined organic layers washed with H2O (1×20 mL) dried over Na2SO4 concentrated
ソース ID: ord-64474ff9992e45518168107afa9f587c反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-8f133474bd3b4b51ad5da2956d77a7b9反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To 4-bromo-1-(difluoromethoxy)-2-methylbenzene (2.36 g, 10.00 mmol) in toluene (50 mL) was added cis-2,6-dimethylpiperazine (5 g, 58.14 mmol), Pd(OAc)2 (120 mg, 0.53 mmol), BINAP (380 mg, 0.61 mmol), and t-BuOK (2.2 g, 19.64 mmol). The resulting solution was stirred for 4 hours at 80° C. The solution was cooled to room temperature and washed with H2O (2×50 mL), dried over Na2SO4, concentrated, and purified by silica gel column chromatography (10:1 CH2Cl2/MeOH) to give 1.1 g (41%) of 1-(4-(difluoromethoxy)-3-methylphenyl)-3,5-dimethylpiperazine. The solution was cooled to room temperature washed with H2O (2×50 mL) dried over Na2SO4 concentrated purified by silica gel column chromatography (10:1 CH2Cl2/MeOH)
ソース ID: ord-5c3bc382159b40b384bb156f94513bb8反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirred solution of 4-amino-1-difluoromethoxy-2-methyl-benzene (5 g, 28.90 mmol) in HBr (20 mL) and water (20 mL) at 0° C. was added a solution of sodium nitrite (2.07 g, 30.00 mmol) in H2O (10 ml) dropwise over a period of 20 minutes. After the addition was complete, the reaction mixture was stirred for 30 minutes at 0° C. Copper (I) bromide (4 g, 27.87 mmol) was then added and the mixture was heated at 60° C. for 30 minutes. The resulting solution was extracted with EtOAc (3×50 mL) and the combined organic layers washed with H2O (1×20 mL), dried over Na2SO4 and concentrated to provide 2.5 g (37%) of 4-bromo-1-(difluoromethoxy)-2-methylbenzene. After the addition the mixture was heated at 60° C. for 30 minutes The resulting solution was extracted with EtOAc (3×50 mL) the combined organic layers washed with H2O (1×20 mL) dried over Na2SO4 concentrated
ソース ID: ord-53a4e676e9af458f8933b289d9414ad9反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To 4-bromo-1-(difluoromethoxy)-2-methylbenzene (2.36 g, 10.00 mmol) in toluene (50 mL) was added cis-2,6-dimethylpiperazine (5 g, 58.14 mmol), Pd(OAc)2 (120 mg, 0.53 mmol), BINAP (380 mg, 0.61 mmol), and t-BuOK (2.2 g, 19.64 mmol). The resulting solution was stirred for 4 hours at 80° C. The solution was cooled to room temperature and washed with H2O (2×50 mL), dried over Na2SO4, concentrated, and purified by silica gel column chromatography (10:1 CH2Cl2/MeOH) to give 1.1 g (41%) of 1-(4-(difluoromethoxy)-3-methylphenyl)-3,5-dimethylpiperazine. The solution was cooled to room temperature washed with H2O (2×50 mL) dried over Na2SO4 concentrated purified by silica gel column chromatography (10:1 CH2Cl2/MeOH)
ソース ID: ord-d301260570764575b6df36e154dfc5aePubChem References
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