関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | Ethyl 5-nitro-1H-indole-2-carboxylate | HCID 280312 | — |
| 溶媒 | Methanol tetrahydrofuran water | HCID 21892291 | — |
| 生成物 | 5-Nitroindole-2-carboxylic acid | HCID 351291 | — |
反応手順
LiOH.H2O (1.06 g, 46.2 mmol, 2.1 eq.) was added to a suspension of 5-nitro-1H-indole-2-carboxylic acid ethyl ester (II) (5.15 g, 22 mmol, 1 eq.) in THF/MeOH/H2O 1:1:2 (180 ml). The final suspension turned to dark yellow and was stirred at 25° C. After 30 min the solubilization was complete and total conversion was achieved after 6 hours. The reaction mixture was cooled to 0° C. and quenched with HCl 2N until the solution reached pH 5. Organic volatiles were removed under reduced pressure and the white precipitate was filtered and dried to give the compound of formula (III). Yield=4.53 g (quantitative).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08207165B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-0fc560e3f5c74fd9bd4f1d068875e49a |
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| 出典メモ | uspto-grants-2012_06 |
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