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2,2-Dimethyl-1,3-propanediamine → HCID 18353695、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2-Dimethyl-1,3-propanediamine | HCID 81770 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chloro-4-methoxyquinoline | HCID 12369166 | — |
| 反応物 | 1,1-Propanediamine | HCID 14954072 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ammonia | HCID 222 | — |
| 生成物 | HCID 18353695 | HCID 18353695 | 45.1% |
反応手順
A mixture of 2-chloro-4-methoxyquinoline (0.63 g, 3.25 mmol) and 2,2-dimethyl-1,3-propanediamine (2.00 g, 19.5 mmol) was stirred for 16 h at 75° C. in a sealed propanediamine (2.00 g, 19.5 mmol) was stirred for 16 h at 75° C. in a sealed NaHCO3 and ethyl acetate. The organic layer was dried (MgSO4) and concentrated onto silica, then chromatographed eluting with 5% then 10% methanol/CH2Cl2+0.5% 880 aqueous ammonia to give the title compound as a white solid (0.19 g, 23%). δH (CDCl3) 0.99 (6H, s, C(CH3)2), 2.57 (2H, s, 2′-H), 3.41 (2H, s, 4′-H), 3.96 (3H, s, OCH3), 5.98 (1H, s, 3-H), 7.12-7.93 (4H, m, ArH). MS (ES+) 260 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06320051B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-b3e0f94bcec74bcd934eb12c62f59691 |
| 出典メモ | uspto-grants-2001_11 |