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Hexane → tert-Butyl 3-ethynylpiperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | tert-Butyl 3-(2,2-dibromovinyl)piperidine-1-carboxylate | HCID 86615128 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-Butyl 3-ethynylpiperidine-1-carboxylate | HCID 21963855 | 93% |
反応手順
To a solution of 3-(2,2-Dibromo-vinyl)-piperidine-1-carboxylic acid tert-butyl ester (0.15 g, 0.42 mmol) in THF (1 ml) wad added at −78° C., 0.5 ml of n-BuLi 2.5 M in hexane (1.23 mmol). After 1 h at −78° C., the reaction mixture was quenched with 1 ml of water and the aqueous phase was extracted with AcOEt. The combined organic phase was dried over K2CO3, filtered and evaporated to give 80 mg (93%) of 3-Ethynyl-piperidine-1-carboxylic acid tert-butyl ester as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07834035B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-bb934716e89d4c329cbf7dae1075806f |
| 出典メモ | uspto-grants-2010_11 |