反应 #3860034
相关文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-86ca01e3fa2e476f9ff93e4c321a4ad8暂无可渲染的结构数据
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12 条反应 · 12 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-86ca01e3fa2e476f9ff93e4c321a4ad8反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-63d7a9aac2dc452fa7cb74d36b28957f反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Then, the solution is concentrated under reduced pressure the residue is dissolved in THF (100 mL) The resulting solution is cooled in an ice-bath LiBH4 (3.4 g) is added in portions The cooling bath is removed the mixture is stirred at room temperature for 1 h The reaction mixture is diluted with THF treated with 0.1 M hydrochloric acid Then, the organic layer is separated the aqueous layer is extracted with ethyl acetate The combined organic layers are dried (Na2SO4) the solvent is evaporated under reduced pressure
来源 ID: ord-d1edf4a6421e46c9baa35d19fc06abf7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-a212c4325e9043fb8a7a41eaedec2983反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-7688fa39bab94122a6c9be36a60b16b2反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-7688fa39bab94122a6c9be36a60b16b2反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Then, the solution is concentrated under reduced pressure the residue is dissolved in THF (100 mL) The resulting solution is cooled in an ice-bath LiBH4 (3.4 g) is added in portions The cooling bath is removed the mixture is stirred at room temperature for 1 h The reaction mixture is diluted with THF treated with 0.1 M hydrochloric acid Then, the organic layer is separated the aqueous layer is extracted with ethyl acetate The combined organic layers are dried (Na2SO4) the solvent is evaporated under reduced pressure
来源 ID: ord-5d971f84d0ad41338b8b27629245dd72反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-e5567449752e4d15be6790955f57f084反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Then, the solution is concentrated under reduced pressure the residue is dissolved in THF (100 mL) The resulting solution is cooled in an ice-bath LiBH4 (3.4 g) is added in portions The cooling bath is removed the mixture is stirred at room temperature for 1 h The reaction mixture is diluted with THF treated with 0.1 M hydrochloric acid Then, the organic layer is separated the aqueous layer is extracted with ethyl acetate The combined organic layers are dried (Na2SO4) the solvent is evaporated under reduced pressure
来源 ID: ord-ad2ed7ffac5a46c2b080c82832390b4b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Thionyl chloride (13 mL) is added to a suspension of 4-bromo-3-hydroxymethyl-1-iodo-benzene (47.0 g) in dichloromethane (100 mL) containing DMF (0.1 mL). The mixture is stirred at ambient temperature for 3 h. Then, the solvent and the excess reagent is removed under reduced pressure. The residue is triturated with methanol and dried. Then, the solvent and the excess reagent is removed under reduced pressure The residue is triturated with methanol dried
来源 ID: ord-e5567449752e4d15be6790955f57f084反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Then, the solution is concentrated under reduced pressure the residue is dissolved in THF (100 mL) The resulting solution is cooled in an ice-bath LiBH4 (3.4 g) is added in portions The cooling bath is removed the mixture is stirred at room temperature for 1 h The reaction mixture is diluted with THF treated with 0.1 M hydrochloric acid Then, the organic layer is separated the aqueous layer is extracted with ethyl acetate The combined organic layers are dried (Na2SO4) the solvent is evaporated under reduced pressure
来源 ID: ord-ad2ed7ffac5a46c2b080c82832390b4b反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-86ca01e3fa2e476f9ff93e4c321a4ad8PubChem References
以下资料来自该化合物的公开数据库参考记录。
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