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1,2-Dimethoxyethane → 3-(Propane-2-sulfonylamino-thiophen-2-yl]-biphenyl-4-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 反応物 | Ethyl 4-iodobenzoate | HCID 142891 | — |
| 反応物 | Sodium Carbonate Monohydrate | HCID 2735133 | — |
| 反応物 | Propane-2-sulfonic acid {2-[4-(4,4,5,5-tetramethyl-[1,3,2] dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide | HCID 59747992 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 生成物 | 3-(Propane-2-sulfonylamino-thiophen-2-yl]-biphenyl-4-carboxylic acid ethyl ester | HCID 131726946 | — |
反応手順
Heat in a sealed tube with stirring propane-2-sulfonic acid{2-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-thiophen-3-yl}-amide (0.5 mmol), 4-iodo-benzoic acid ethyl ester (0.75 mmol), 2M Na2CO3 water solution (0.2 mL) and Pd(PPh3)4 (0.05 mmol) in 4.0 ml of an anhydrous DME to 100° C. for 24 h. Evaporate the organic solvent, prior to the addition of water (10 mL). Extract the mixture with dichloromethane (3×20 mL) and dry the combined organic phases (Na2SO4) and concentrate to furnish a crude mixture. Purification by flash chromatography (Silica gel-hexane/EtOAc) yields the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07393868B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-5b7048ec6a9c44d197a51e5820c4c004 |
| 出典メモ | uspto-grants-2008_07 |