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Hydrochloric Acid → 5-(2,2,4-Trimethyl-piperazin-1-ylmethyl)-pyridin-2-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | [5-(2,2,4-Trimethyl-piperazin-1-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester | HCID 66914640 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-(2,2,4-Trimethyl-piperazin-1-ylmethyl)-pyridin-2-ylamine | HCID 66914602 | 75% |
反応手順
A mixture of [5-(2,2,4-trimethyl-piperazin-1-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester (Step 110.2) (1.94 g, 5.8 mmol), a 4 N solution of HCl in dioxane (20 mL) and MeOH (5 mL) was stirred for 12 h at rt and concentrated. The residue was purified by silica gel column chromatography (DCM/NH3aq, 99:1→DCM/MeOH/NH3aq, 95:4:1) to afford 1.02 g of the title compound as a white solid. Title compound: ESI-MS: 235.2 [M+H]+; TLC: Rf=0.11 (DCM/MeOH, 9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08273882B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-49478071dbb442fbaf1fe67bd3f52271 |
| 出典メモ | uspto-grants-2012_09 |