化工社化工社 化学情報印刷レポート · 研究参考用
2-Amino-2-methyl-1,3-propanediol → 2-(1-hydroxymethyl-1-methyl-2-hydroxyethyl amino)-4-(4-fluoro-2-methylphenyl)-8-(2,6-difluorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-2-methyl-1,3-propanediol | HCID 1531 | — |
| 反応物 | 8-(2,6-difluoro-phenyl)-4-(4-fluoro-2-methyl-phenyl)-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 59639554 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(1-hydroxymethyl-1-methyl-2-hydroxyethyl amino)-4-(4-fluoro-2-methylphenyl)-8-(2,6-difluorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 59639563 | — |
反応手順
The product of Example 48 (300 mg, 0.67 mmol) and 2-amino-2-methyl-1,3-propanediol (158 mg, 1.5 mmol) were combined in THF (10 mL) and stirred under Ar at 50° for 3 days. The solvents were removed in vacuo, and the residue was flash chromatographed with 0-25% EtOAc/CH12Cl2. Recrystallization from CH2Cl2/hexane gave the title compound as a white crystalline solid. mp 158-160°, LC MS m/z=471 (MH+) Retention time=1.75 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07314934B2 |
| 出典データセット | uspto-grants-2008_01 |
| ORD ID | ord-907848b14ee54855be51fe3adb4040ea |
| 出典メモ | uspto-grants-2008_01 |