化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → (e)-3-[6-[n-(Methoxycarbonylmethyl)amino]pyridin-3-yl]acrylic acid hydrochloride salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | tert-butyl (E)-3-[6-[N-(methoxycarbonylmethyl)amino]pyridin-3-yl]acrylate | HCID 66905699 | — |
| 生成物 | (e)-3-[6-[n-(Methoxycarbonylmethyl)amino]pyridin-3-yl]acrylic acid hydrochloride salt | HCID 66905135 | 100% |
反応手順
A solution of 50% TFA in CH2Cl2 (75 mL) was added to tert-butyl (E)-3-[6-[N-(methoxycarbonylmethyl)amino]pyridin-3-yl]acrylate (5.20 g, 17.8 mmole). The reaction was stirred at room temperature for 45 min then was concentrated under vacuum. The residue was taken up in 4.0 N HCl in dioxane (75 mL), stirred for 5 min, then concentrated to dryness under vacuum. The remaining solid was triturated with 1:1 Et2O/petroleum ether, filtered and dried under vacuum to give the title compound (4.87 g, 100%) as a white solid: MS (ES) m/e 237.2 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741339B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-2922442bd0ed47cc8e2481062f9bc4a5 |
| 出典メモ | uspto-grants-2010_06 |