関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentafluoropropionic acid | HCID 62356 | — |
| 反応物 | Methyl 3,4-diamino-5-methylthiophene-2-carboxylate | HCID 18693138 | — |
| 生成物 | HCID 178499322 | HCID 178499322 | — |
反応手順
A mixture of methyl 3,4-diamino-5-methylthiophene-2-carboxylate (1.0 g) in pentafluoropropionic acid (8.9 g) was stirred at 100° C. for 6 hr. The reaction solution was concentrated to dryness and the residue was suspensed in water. The mixture was made basic with aqueous solution of K2CO3, followed by extraction with ethyl acetate. The organic layer was washed with water, dried and concentrated to dryness. The residue was purified by silica gel column chromatography to give crystals. Recrystallization from isopropyl ether-hexane gave colorless plates (0.86 g, 51%). m.p. 156°-157° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05463073 |
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| 出典データセット | uspto-grants-1995_10 |
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| ORD ID | ord-0b542faa7968475393bf06b11052ba00 |
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| 出典メモ | uspto-grants-1995_10 |
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