関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributyltin Chloride | HCID 15096 | — |
| 反応物 | 5-(difluoromethoxy)-3-iodo-1-methyl-1H-indazole | HCID 71279544 | — |
| 反応物 | HCID 178418918 | HCID 178418918 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(Difluoromethoxy)-1-methyl-3-(tributylstannyl)-1H-indazole | HCID 71279627 | — |
反応手順
5-(Difluoromethoxy)-3-iodo-1-methyl-1H-indazole (0.265 g, 818 μmol) was dissolved in THF (3.00 mL). The colorless solution was cooled to −16° C. (NaCl/ice bath) then isopropylmagnesium chloride (2M in THF, 458 μL, 916 μmol) added dropwise at −16° C. The reaction mixture was stirred at −16° C. for 20 min then tributylchlorostannane (306 mg, 255 μL, 940 μmol) was added slowly. The reaction mixture was warmed to 25° C. and stirred for 1.5 h. The reaction mixture was quenched with saturated ammonium chloride solution, extracted with dichloromethane (3×30 mL), organics dried over MgSO4 and concentrated to a yellow oil. The residue was dried under high vacuum and taken into next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08658646B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-ade00f536a8e4f59869b3e4da9cb8039 |
|---|
| 出典メモ | uspto-grants-2014_02 |
|---|