化工社化工社 化学情報印刷レポート · 研究参考用
1H-Pyrazol-3-amine, 5-methyl- → 1-Benzothiazol-6-yl-3-{4-[(5-methyl-1H-pyrazol-3-ylamino)-methyl]-pyridin-3-yl}-imidazolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1H-Pyrazol-3-amine, 5-methyl- | HCID 93146 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 3-(3-Benzothiazol-6-yl-2-oxo-imidazolidin-1-yl)-pyridine-4-carbaldehyde | HCID 59636272 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Benzothiazol-6-yl-3-{4-[(5-methyl-1H-pyrazol-3-ylamino)-methyl]-pyridin-3-yl}-imidazolidin-2-one | HCID 49872742 | 7.7% |
反応手順
3-(3-benzothiazol-6-yl-2-oxo-imidazolidin-1-yl)-pyridine-4-carbaldehyde (I-177b: 100 mg, 0.308 mmol) was reacted with NaBH(OAc)3 (131 mg, 0.616 mmol), 5-methyl-1H-pyrazol-3-ylamine (40 mg, 0.370 mmol) and acetic acid (10 mL) to afford the crude product. Purification by column chromatography on silica gel (5% MeOH in CHCl3), followed by preparative HPLC afforded 4 mg of the product (7.7% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE045173E1 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-5dba349b9d784c1ca873e255b4f56aa7 |
| 出典メモ | uspto-grants-2014_09 |