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Hydrochloric Acid → (R)-ethyl 3-amino-4-(5'-fluoro-2'-methoxybiphenyl-4-yl)butanoate hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | (R)-ethyl 3-(tert-butoxycarbonylamino)-4-(5'-fluoro-2'-methoxybiphenyl-4-yl)butanoate | HCID 59607779 | — |
| 生成物 | (R)-ethyl 3-amino-4-(5'-fluoro-2'-methoxybiphenyl-4-yl)butanoate hydrochloride | HCID 68423640 | — |
反応手順
A solution of (R)-ethyl 3-(tert-butoxycarbonylamino)-4-(5′-fluoro-2′-methoxybiphenyl-4-yl)butanoate, (2.86 g, 6.62 mmol) in 4M HCl in 1,4-dioxane (33.1 ml, 132 mmol) is stirred at room temperature. After stirring for 1 hour, the reaction mixture is concentrated under reduced pressure to give (R)-ethyl 3-amino-4-(5′-fluoro-2′-methoxybiphenyl-4-yl)butanoate hydrochloride salt (2.44 g). HPLC retention time=1.46 minutes (condition A); MS (m+1)=332.3; 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.15 (t, J=6.4 Hz, 3 H) 2.66-2.77 (m, 1 H) 2.78-2.91 (m, 1 H) 2.94-3.10 (m, 1 H) 3.42-3.53 (m, 1 H) 3.67 (s, 3 H) 3.83-3.96 (m, 1 H) 4.07 (q, J=6.8 Hz, 2 H) 6.77-6.84 (m, 1 H) 6.87-6.96 (m, 2 H) 7.23 (d, J=7.1 Hz, 2 H) 7.38 (d, J=7.1 Hz, 2 H) 8.64 (br. s., 2 H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822534B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-84d02c4cba8c4917a5745e4d51dd4f9e |
| 出典メモ | uspto-grants-2014_09 |