関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(2-methoxy-2-methyl-propyl)-3-nitro-1H-pyrazole | HCID 66899320 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 66899934 | HCID 66899934 | 71% |
反応手順
In a Parr shaker bottle was placed 1-(2-methoxy-2-methyl-propyl)-3-nitro-1H-pyrazole (1.33 g, 6.68 mmol), 10% palladium on activated carbon (135 mg) and ethanol (50 mL). The bottle was then placed on the Parr shaker at 50 psi of hydrogen pressure for 2 h. The reaction was then filtered through a pad of celite and washed with ethanol and concentrated in vacuo with silica gel (3 g) and purified on Biotage Flash chromatography system (40S column, silica gel, 5% methanol/ethyl acetate) to afford 1-(2-methoxy-2-methyl-propyl)-1H-pyrazol-3-ylamine (802 mg, 71%) as a colorless oil: ES-HRMS m/z calculated for C23H33N3O5S [M+H]+ 464.2214, observed 464.2208; 1H NMR (300 MHz, DMSO-d6) δ ppm 1.04 (s, 6H), 3.13 (s, 3H), 3.80 (s, 2H), 4.48 (brs, 2H), 5.38 (d, J=2.3 Hz, 1H), 7.21 (d, J=2.3 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07741327B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-7de330317f274970a2829688ed8377e8 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|