関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Borane | HCID 6331 | — |
| 反応物 | Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate | HCID 21097379 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Hydrazinyl-1-methylpiperidine | HCID 10920535 | 81.8% |
反応手順
A solution of 1 M borane in THF (30 mL) was added to solid 2.80 g (12.3 mmol) of tert-butyl N′-(1-Methyl-piperidin-4-ylidene)-hydrazinecarboxylate. The mixture was stirred under N2 for 16 h when 40 mL of 6M HCl was carefully added. The mixture was heated to 60° C. for 30 min. The mixture was concentrated in vacuo at ambient temperature for 2 days. Petroleum ether (200 mL) and powdered NaOH (5 g) were added, and the mixture was stirred manually for 30 min. The mixture was dried with MgSO4, filtered, and carefully concentrated to give 1.3 g of (1-methyl-piperidin-4-yl)-hydrazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07514458B2 |
|---|
| 出典データセット | uspto-grants-2009_04 |
|---|
| ORD ID | ord-7b6ff192016d496fbf220b53c76b1f33 |
|---|
| 出典メモ | uspto-grants-2009_04 |
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