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Methylamine → Ethyl 4-methyl-2-(N'-methylureido)thiophene-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl 2-amino-4-methylthiophene-3-carboxylate | HCID 521132 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 4-methyl-2-(N'-methylureido)thiophene-3-carboxylate | HCID 15085569 | — |
反応手順
To a stirred ice-cooled solution of ethyl 2-amino-4-methyl-thiophene-3-carboxylate (1,85 g, 10 mmole) and triethyl amine (1,4 ml, 10 mmol) in dry tetrahydrofuran (50 ml) was added dropwise a phosgene solution (11 mmol, in toluene). The mixture was thereafter heated to reflux for 30 min, then cooled to room temperature and exposed to a gaseous stream of methylamine for 5 min. After additional stirring for 15 min, the mixture was filtered and the filtrate was evaporated to give the title compound as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04866065 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-da50db23273a4eb0b833d8c5bb1271dc |
| 出典メモ | uspto-grants-1989_09 |