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Borane;tetrahydrofuran → Tert-butyl 3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 反応物 | Tert-butyl 3-(pyridin-3-ylcarbamoyl)piperazine-1-carboxylate | HCID 59671553 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate | HCID 59671589 | — |
反応手順
Borane-THF complex (1.0 M solution in THF, 3.4 mL, 3.4 mmol) was added to a solution of tert-butyl 3-(pyridin-3-ylcarbamoyl)piperazine-1-carboxylate (522 mg, 1.70 mmol) in THF (4 mL). The reaction mixture was heated to reflux for 5 h. Upon cooling to rt, the reaction mixture was carefully quenched by the dropwise addition of MeOH. After gas evolution ceased, MeOH (10 mL) was added, and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure, yielding the title compound which was used without further purification. LC-MS: RT=2.90 min, [M+H]+=293.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822472B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-fa00b21b9f744c02a7a0d1a7d17a6886 |
| 出典メモ | uspto-grants-2014_09 |