関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | N'-[3-tert-butyl-1-(oxan-2-ylmethyl)pyrazol-5-yl]-N,N-dimethylmethanimidamide | HCID 87440113 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Tert-butyl-1-((tetrahydro-2h-pyran-2-yl)methyl)-1h-pyrazol-5-amine | HCID 67544533 | — |
反応手順
To a solution of Example 63B (0.9 g, 3.1 mmol) in dioxane (10 mL) were added hydrazine (0.12 mL, 3.7 mmol, Aldrich) and acetic acid (0.35 mL, 6.2 mmol). After stirring at 85° C. for 16 hours, the reaction mixture was cooled and quenched with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to provide the title compound. MS (APCI+) m/z 238 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08492371B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-9f1e66612f644f2380608be7ebeefcdd |
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| 出典メモ | uspto-grants-2013_07 |
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