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Diisopropylethylamine → 5-Methyl-2-{4-[(2-methyl-pyrimidin-5-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | (2-Methylpyrimidin-5-yl)methanamine | HCID 21294601 | — |
| 反応物 | 2-(4-Chloro-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-methylbenzonitrile | HCID 59840688 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Methyl-2-{4-[(2-methyl-pyrimidin-5-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile | HCID 25059289 | — |
反応手順
A reaction mixture of 2-(4-chloro-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-5-methylbenzonitrile (400 mg, 1.41 mmol) and (2-methylpyrimidin-5-yl)methanamine (400 mg, 3.25 mmol) in acetonitrile (3 mL) and N,N-diisopropylethylamine (1.5 mL, 8.6 mmol) was subjected to microwave irradiation at 185° C. for 2.5 h. The reaction mixture was concentrated and purified by preparative HPLC (100×20.2 mm, C18 column; 40-60% CH3CN-water [10 mM Et2NH]) to yield a light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076345B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-a5ac386a0c3f4ffbbb0a600279d240ec |
| 出典メモ | uspto-grants-2011_12 |