1,4-Dioxane hydrochloride → HCID 66742844、化合物
反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[C:8][C:9]1[CH:10]=[C:11]([CH2:15][CH2:16][CH2:17][NH:18]C(=O)OC(C)(C)C)[CH:12]=[CH:13][CH:14]=1.[ClH:26].O1CCOCC1>C(Cl)Cl>[ClH:26].[CH3:1][O:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[C:8][C:9]1[CH:10]=[C:11]([CH2:15][CH2:16][CH2:17][NH2:18])[CH:12]=[CH:13][CH:14]=1参加物
4
実験手順
tert-Butyl 3-(3-(6-methoxyhex-1-ynyl)phenyl)propylcarbamate was deprotected following the method used in Example 13 except that CH2Cl2 was used as a cosolvent in the reaction (HCl-dioxane solution: CH2Cl2 7:5). Purification by prep HPLC (Method 2P) gave 3-(3-(6-methoxyhex-1-ynyl)phenyl)propan-1-amine hydrochloride as an off white solid. Yield (0.050 g, 30%): 1H NMR (400 MHz, CDCl3) δ 8.37 (br s, 3H), 7.10-7.24 (m, 4H), 4.02 (t, J=6.4 Hz, 2H), 3.78 (s, 3H), 2.98 (t, J=7.6 Hz, 2H), 2.69 (t, J=7.6 Hz, 2H), 2.44 (t, J=7.6 Hz, 2H), 2.04-2.12 (m, 2H), 1.82-1.89 (m, 2H), 1.63-1.73 (m, 2H).
後処理
- customPurification by prep HPLC (Method 2P)
出典と根拠
- ORDレコード
- ord-38c0c3f3ca8448a79d636ea2a238cb5f
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716529B2
反応ノート
読み込み中…