関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Chloro-3-hydrazinyl-4-methylpyridazine | HCID 11446490 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Chloro-3,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazine | HCID 15503806 | 85.9% |
反応手順
6-chloro-3-hydrazinyl-4-methylpyridazine (Step 111.1) (721 mg, 4.55 mmol) was dissolved in AcOH (15 mL, 262 mmol) and the resulting mixture was heated up and stirred at 115° C. for 1 hr. The reaction was cooled down to RT, diluted with CH2Cl2 and poured into a saturated aq. NaHCO3 solution. The aq. layer was extracted with CH2Cl2. The combined organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure to afford the title product (752 mg, 3.91 mmol, 84% yield) as grey solid. tR: 0.59 min (LC-MS 2); ESI-MS: 183 [M+H]+ (LC-MS 2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08975417B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-106a0be2b2bf43a3ab0a6fdcc0b1ced0 |
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| 出典メモ | uspto-grants-2015_03 |
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