関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 1-isopentyl-4-nitro-1H-pyrrole-2-carboxylate | HCID 67183320 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(3-methyl-butyl)-4-nitro-1H-pyrrole-2-carboxylic acid | HCID 21880772 | 100.7% |
反応手順
1-(3-Methyl-butyl)-4-nitro-1H-pyrrole-2-carboxylic acid ethyl ester (1.44 g,) was dissolved in 50 ml of methanol and 25 ml of 20% aqueous NaOH was added. The reaction mixture was stirred at 50° C. for 1.5 h until there was no starting material checked by TLC. The reaction mixture was concentrated to about 20 ml, 200 ml of water was added. The resulting solution was neutralized with 5 M hydrochloric acid to pH 2 and the precipitates formed were collected by filtration, washed with water and dried to give 1-(3-methyl-butyl)-4-nitro-1H-pyrrole-2-carboxylic acid (1.29 g, 99%). 1H NMR (DMSO-d6) δ13.12 (br. s, 1H), 8.27 (d, 1H), 7.26 (d, 1H), 4.36 (t, 2H), 1.59 (dd, 2H), 1.50 (dt, 1H), 0.88 (d, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06849713B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-5ae4b7815f014a428f4a5bf826048932 |
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| 出典メモ | uspto-grants-2005_02 |
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