関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isopropyl 5-amino-2-chlorobenzoate | HCID 369590 | — |
| 反応物 | 2,4,5-Trimethyl-3-furancarbonyl chloride | HCID 14535934 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Isopropyl 2-chloro-5-[(2,4,5-trimethylfuran-3-carbonyl)amino]benzoate | HCID 507312 | 42.6% |
反応手順
A solution of 2,4,5-trimethyl-3-furancarbonyl chloride (7.8 g, 0.045 mole) in toluene (25 ml) was added to 1-methylethyl 5-amino-2-chlorobenzoate (10.6 g, 0.050 mole) and triethylamine (6 g) in toluene (25 ml). The mixture was warmed to 60° C. for about 1 hour, then washed in sequence with dilute hydrochloric acid, water, aqueous 5% sodium bicarbonate and water. The solution was dried with magnesium sulfate, filtered and evaporated. The residue was crystallized from toluene/petroleum ether to give 6.7 g of a pale yellow solid, m.p. 83°-85° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05268389 |
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| 出典データセット | uspto-grants-1993_12 |
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| ORD ID | ord-75503f14faa44da6902649854861f5a8 |
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| 出典メモ | uspto-grants-1993_12 |
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