関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Isopropylhydrazine hydrochloride | HCID 85573 | — |
| 反応物 | 4-Ethoxy-3-oxobutanenitrile | HCID 57516910 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-[(Ethyloxy)methyl]-1-(1-methylethyl)-1H-pyrazol-5-amine | HCID 57516909 | 65.6% |
反応手順
To a 25 mL round bottom was added 4-(ethyloxy)-3-oxobutanenitrile (550 mg, 4.33 mmol), isopropyl hydrazine hydrochloride (478 mg, 4.33 mmol), and HCl (2.163 mL, 4.33 mmol) in Ethanol (10 mL). The reaction mixture was stirred at the room temperature overnight. The reaction mixture was then evaporated, and partitioned between 20 mL of ethyl acetate and 20 mL of 1 M Na2CO3. The organic layer was washed with brine, filtered and evaporated. 3-[(Ethyloxy)methyl]-1-(1-methylethyl)-1H-pyrazol-5-amine (520 mg, 2.84 mmol, 65.6% yield) was isolated as yellow oil. The product was used in the next step without further purification. 1H NMR (400 MHz, DMSO-d6) ppm 1.09 (t, J=7.07 Hz, 3 H) 1.26 (d, J=6.57 Hz, 6 H) 3.40 (q, J=6.91 Hz, 2 H) 4.16 (s, 2 H) 4.32 (quin, J=6.57 Hz, 1 H) 5.06 (s, 2 H) 5.22 (s, 1 H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09446034B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-939fca259526463da317d6465f6dac9e |
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| 出典メモ | uspto-grants-2016_09 |
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