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Acetic Acid → (R)-2-(4-cyano-3-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-4-methylpentanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Methylisothiazol-5-ylamine hydrochloride | HCID 2723918 | — |
| 反応物 | (R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide | HCID 67509019 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | (R)-2-(4-cyano-3-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-4-methylpentanamide | HCID 67510110 | 30.9% |
反応手順
To a solution of (R)-2-(4-cyano-3,5-difluorophenylamino)-4-methylpentanamide (92 mg, 0.34 mmol) and 5-amino-3-methylisothiazole hydrochloride (70 mg, 0.46 mmol) in DMSO (2 mL), NaH (60% in mineral oil, 80 mg, 2.00 mmol) was added. H2 gas evolved. The mixture was stirred at 130 C for 1 h. After being acidified with HOAc (1.0 mL), the mixture was purified by HPLC to give (R)-2-(4-cyano-3-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-4-methylpentanamide (38 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09359375B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-a3c2c777863647fa84351519fb308c3b |
| 出典メモ | uspto-grants-2016_06 |