化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → (R)-2-(4-cyano-2-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 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | 3-Methylisothiazol-5-ylamine hydrochloride | HCID 2723918 | — |
| 反応物 | (R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-4-methylpentanamide | HCID 67508329 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (R)-2-(4-cyano-2-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-4-methylpentanamide | HCID 67508594 | — |
反応手順
A mixture of (R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-4-methylpentanamide (175 mg, 0.533 mmol), 5-amino-3-methylisothiazole hydrochloride (97 mg, 0.644 mmol), BINAP (50 mg, 0.080 mmol), Pd(OAc)2 (35 mg, 0.156 mmol) and K2CO3 (250 mg, 1.81 mmol) in dioxane (4 mL) was degassed with Ar, then was stirred at 120 C for 18 h. Water and EtOAc were added. After being filtered, the filtrate was washed with water, dried over Na2SO4, concentrated in vacuo to give (R)-2-(4-cyano-2-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-4-methylpentanamide as a crude residue.
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-6e10b5c77cd349f7928d905923e9e32f |
| 出典メモ | uspto-grants-2016_06 |