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1-Boc-1-methylhydrazine → methyl 1-(N-tert-butoxycarbonyl-N-methylamino)-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Boc-1-methylhydrazine | HCID 3748280 | — |
| 反応物 | Methyl 3-dimethylamino-2-(2,3,4,5-tetrafluorobenzoyl)acrylate | HCID 53884844 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methyl 1-(N-tert-butoxycarbonyl-N-methylamino)-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate | HCID 18959448 | 62.8% |
反応手順
To methylene chloride (120 ml) solution of methyl 3-dimethylamino -2-(2,3,4,5-tetrafluorobenzoyl)acrylate (13.2 g) was added methylene chloride (12 ml) solution of 1-tert-butoxycarbonyl-1-methylhydrazine (7.59 g) with ice-cooling, and the mixture was stirred for one hour at the same temperature and then for 15 hours at room temperature. The reaction mixture was concentrated under reduced pressure. The residue was triturated with diisopropyl ether (132 ml). The solid formed was taken out by filtration and dried with phosphorus pentaoxide under reduced pressure to obtain methyl 1-(N-tert-butoxycarbonyl-N-methylamino)-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (10.49 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05359066 |
| 出典データセット | uspto-grants-1994_10 |
| ORD ID | ord-cc0b7e2f8d064d019f7c36b789a8aaa5 |
| 出典メモ | uspto-grants-1994_10 |