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2,4,4,6-Tetrabromocyclohexa-2,5-dienone → methyl (2S)-1-(6-bromo-1,3-benzoxazol-2-yl)-2-piperidinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4,4,6-Tetrabromocyclohexa-2,5-dienone | HCID 88433 | — |
| 反応物 | methyl (2S)-1-(1,3-benzoxazol-2-yl)-2-piperidinecarboxylate | HCID 10220819 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methyl (2S)-1-(6-bromo-1,3-benzoxazol-2-yl)-2-piperidinecarboxylate | HCID 9949771 | 95.1% |
反応手順
2,4,4,6-Tetrabromo-2,5-cyclohexadien-1-one (4.7 g) was added to a solution of methyl (2S)-1-(1,3-benzoxazol-2-yl)-2-piperidinecarboxylate (3.0 g) [see Preparation 2] in dichloromethane (60 ml) at −10° C. over a period of 10 minutes. The reaction mixture was then warmed to room temperature and diluted with dichloromethane. The organic layer was washed with saturated sodium hydrogen carbonate, then with 1N sodium hydroxide solution, dried over sodium sulphate and the solvent removed under reduced pressure to afford methyl (2S)-1-(6-bromo-1,3-benzoxazol-2-yl)-2-piperidinecarboxylate (3.7 g) as a purple coloured oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06562964B1 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-d28894faf6d1432a999cc21be042e341 |
| 出典メモ | uspto-grants-2003_05 |