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Diisopropylethylamine → 4-methyl-6-{6-[4-(5-oxo-3-phenyl-4,5-dihydro-1,2,4-triazol-1-yl)-piperidin-1-yl]-pyrimidine-4-carbonyl}-3H-benzoxazol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one | HCID 58181206 | — |
| 反応物 | HCID 135627598 | HCID 135627598 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-methyl-6-{6-[4-(5-oxo-3-phenyl-4,5-dihydro-1,2,4-triazol-1-yl)-piperidin-1-yl]-pyrimidine-4-carbonyl}-3H-benzoxazol-2-one | HCID 135921409 | — |
反応手順
378 mg (1.00 mmol) 5-phenyl-2-piperidin-4-yl-2,4-dihydro-1,2,4-triazol-3-one, 289 mg (1.00 mmol) 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one and 0.348 mL (2.0 mmol) DIPEA were stirred overnight in 10 mL DMF at RT. The mixture was purified by preparative HPLC-MS. The fractions containing the product were combined, the organic solvent was eliminated i. vac. and the aqueous phase remaining was neutralised with a 4N aqueous NaOH solution. The precipitate was suction filtered, washed with water and dried in the CAD.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08629137B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-b2ed7abcd8b94958944d7d065c7cc43e |
| 出典メモ | uspto-grants-2014_01 |