関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | tert-Butyl carbazate | HCID 70091 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-Chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine | HCID 54595607 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | tert-butyl 2-[6-(1-methyl-1H-pyrazol-4-yl)pyridazin-3-yl]hydrazinecarboxylate | HCID 59439328 | — |
反応手順
tert-butyl carbazate, 8.98 g (67.3 mmol) and 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine (11.9 g, 61.1 mmol) were mixed in 1-butanol (245 mL). This mixture was heated till 90° C. and stirred at that temperature for 16 h. The reaction mixture was cooled and water (250 mL) and ethylacetate (250 mL) were added. The biphasic mixture was neutralised with sodium hydrogencarbonate till the pH is 7. Then the organic layer was separated and the water layer was extracted with ethylacetate (250 mL). The combined organic layers were washed once with water (250 mL) and evaporated. The residue was stirred in isopropylether, filtered off and dried under vacuum. Yield: 5.9 g (20.3 mmol; 33%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08629144B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-8bdeb6c41d014b839912adece49a875b |
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| 出典メモ | uspto-grants-2014_01 |
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