関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 3-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-2-carboxylate | HCID 312340 | — |
| 反応物 | Chloroformamidinium chloride | HCID 3084509 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | HCID 178508937 | HCID 178508937 | 95.5% |
反応手順
A 48 mL sealed tube was charged with 3-amino-4,5,6,7-tetrahydro-benzo[b]thiophene-2-carboxylic acid ethyl ester (2.8 g, 12.3 mmol), chloroformamidine hydrochloride (2.0 g, 17.2 mmol), and diethylene glycol dimethyl ether (24.6 mL). The tube was sealed and heated to 160° C. for 12 h with vigorous stirring. Filtration afforded the desired compound as a beige solid (2.6 g). MS: No signal. 1H NMR (400 MHz, d6-DMSO) δ ppm 2.84-2.73 (m, 2H), 2.58-2.51 (m, 2H), 1.89-1.70 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193178B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-f0a4c69cac35436a9c47ea9285d5f640 |
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| 出典メモ | uspto-grants-2012_06 |
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