反応 #4027695
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-9d8334112fc943508b5b40c5b63c3000表示可能な構造データがありません
COC1=CC(=C(C=C1Cl)Cl)Br製品情報
1-bromo-2,4-dichloro-5-methoxybenzene (CAS 174913-22-5) 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 19607721
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-9d8334112fc943508b5b40c5b63c3000反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-c3f8cc4f336b426893ca41899a6ba0d9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-c3f8cc4f336b426893ca41899a6ba0d9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)j (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-d0aa79fbcbb84cd4ae226e9a8cc7e2cf反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-ebd55804ccdd46bc9dd1df4e506352e1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-ebd55804ccdd46bc9dd1df4e506352e1反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-9d8334112fc943508b5b40c5b63c3000反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-a8fa763331de44feadc9549c1fb9b0b8反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1 g of 5-bromo 2-chloro anisole and 0.66 g of N-chloro succinimide in 10 ml of acetic acid is heated at 90° C. for 20 hours. The reaction medium is poured into water, extraction is carried out with methylene chloride. The organic phase is washed with a saturated aqueous solution of sodium bicarbonate, dried over magnesium sulphate and evaporated under reduced pressure. 1.15 g of sought product is obtained. The organic phase is washed with a saturated aqueous solution of sodium bicarbonate dried over magnesium sulphate evaporated under reduced pressure
ソース ID: ord-090fb9c9f5314177b4b0d9c9efade134反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-a314c24b7f1841caa3d0bebc1f786910反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-c3f8cc4f336b426893ca41899a6ba0d9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)j (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification. The mixture was heated under reflux for 4 h under Ar The solid was filtered off the filtrate washed with brine (1×100 mL) The organic solution was separated dried (Na2SO4) The solvent was removed in vacuo The crude product was used for next reaction without purification
ソース ID: ord-d0aa79fbcbb84cd4ae226e9a8cc7e2cfPubChem References
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