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Sodium Bicarbonate → HCID 178478381、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chlorophenylboronic acid | HCID 2734322 | — |
| 反応物 | Potassium phenoxide | HCID 23670670 | — |
| 反応物 | HCID 178478383 | HCID 178478383 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178478381 | HCID 178478381 | 63% |
反応手順
To (2-Chloro-6-iodo-quinazolin-4-yl)-(5-cyclopropyl-2H-pyrazol-3-yl)-amine (100 mg, 0.243 mmol) and 2-chlorophenyl boronic acid (57 mg, 0.364 mmol) in DMSO (5 mL, purged with Ar) was added 1.5M potassium phenolate solution (648 μL, 0.97 mmol) and 1,1′bis(diphenylphosphino)ferrocene palladium chloride, complex with dichloromethane (27 mg) and the solution was heated to 60 C in a sealed tube. After 1 hr, solution was poured into sat. NaHCO3 resulting in a yellow solid that was colleted by filtration. Flash chromatography (1–4% methanol in dichloromethane) to give: 73 mg (63% yield). LCMS m/e: 396.2 (M+H), 394.2 (M−H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07262200B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-345d575cc3c2465ca5fbb3eadb937295 |
| 出典メモ | uspto-grants-2007_08 |