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Sodium Iodide → HCID 19784154、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Dichlorodimethylsilane | HCID 6398 | — |
| 反応物 | 1-(2-Ethyl-6,8-dimethylimidazo[1,2-b]pyridazin-3-yl)-1-(4-hydroxyphenyl)methanol | HCID 19784150 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 19784154 | HCID 19784154 | 90% |
反応手順
To a stirred suspension of 2.607 g (8.8 mmol) of the product of Step D and 5.257 g (35.1 mmol) of sodium iodide in 12 mL of acetonitrile was added 2.13 mL (17.5 mmol) of dichlorodimethylsilane via syringe under a nitrogen atmosphere. The reaction mixture which immediately darkened was stirred for 20 min at room temperature, then partitioned between EtOAc and brine. The organic layer was washed with aqueous sodium bicarbonate, 10% aqueous sodium thiosulfate, then dried (MgSO4), filtered and evaporated. The residue was crystallized from EtOAc-hexane to afford 2.214 g (90%) of the title compound as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05250521 |
| 出典データセット | uspto-grants-1993_10 |
| ORD ID | ord-d465f4fc90ad4e75908f76dba7fa81bb |
| 出典メモ | uspto-grants-1993_10 |