関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | 2-(4-Benzyloxy-phenyl)-ethylamine | HCID 200957 | — |
| 反応物 | Ammonium Sulfate | HCID 6097028 | — |
| 反応物 | HCID 178518044 | HCID 178518044 | — |
| 生成物 | [2-(4-Benzyloxyphenyl)-ethyl]-pteridin-4-yl-amine | HCID 51000640 | 73.8% |
反応手順
To a mixture of pteridin-4-ol (282 mg, 1.9 mmol) and 2-(4-benzyloxyphenyl)-ethylamine (476 mg, 2.1 mmol) and hexamethyldisilazane (5 mL) in a 25 mL round bottom flask, equipped with reflux condenser, drying tube and magnetic stir bar, was added ammonium sulfate (100 mg, 0.76 mmol). The mixture was heated to 114° C. overnight and then the solvent was removed in vacuo. The residue was suspended in H2O and filtered. The filter cake was dissolved in CH2Cl2, dried with Na2SO4, filtered, and concentrated in vacuo to provide [2-(4-benzyloxyphenyl)-ethyl]-pteridin-4-yl-amine as a white solid (501 mg): 1H NMR (300 MHz) δ 9.01 (d, J=1.9 Hz, 1H), 8.81 (s, 1H), 8.61 (d, J=1.9 Hz, 1H), 7.49-7.29 (m, 6H), 7.25-7.15 (m, 3H), 6.96 (dd, J=6.8, 4.8 Hz, 2H), 5.06 (s, 2H), 3.93 (dd, J=13.2, 6.9 Hz, 2H), 3.00 (t, J=7.0 Hz, 2H); ESIMS m/z 358.1 ([M+H]+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08895568B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-77c73c745c1c4686897b5f10ee01b42b |
|---|
| 出典メモ | uspto-grants-2014_11 |
|---|