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 | Ethanol | HCID 702 | — |
| 生成物 | 1-(3-methyl-butyl)-4-nitro-1H-pyrrole-2-carboxylic acid | HCID 21880772 | 95.1% |
反応手順
Ethyl 1-isopentyl-4-nitro-1H-pyrrole-2-carboxylate (2.377 g, 9.329 mmol; see step (i) above) was suspended in ethanol (5 mL), then a solution of NaOH (955 mg dissolved in 20 mL of water) was added. The reaction mixture was reduced by half under reduced pressure at 50° C., and then the cooled solution was extracted with ether. The water layer was cooled to 0° C. then conc. HCl was added dropwise with vigorous stirring until pH 2. The white solid material was filtered off, washed with water, dried at 60° C. under reduced pressure for 2 h then left at room temperature overnight. The product was obtained as white solid (2.008 g, 95% yield), m.p. 154-157° C. [Lit.m.p. 154-156° C.].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07700765B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-fc969097f8e0408eb4811a120b98eae3 |
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| 出典メモ | uspto-grants-2010_04 |
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