関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | m-Ethylbenzaldehyde | HCID 118623 | — |
| 反応物 | 1-Methyl-3-phenyl-1H-1,2,4-triazole | HCID 10877408 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (3-ethylphenyl)(2-methyl-5-phenyl-2H-1,2,4-triazol-3-yl)methanol | HCID 57803786 | 79.5% |
反応手順
To a solution of 1-methyl-3-phenyl-1H-1,2,4-triazole (284 mg, 1.8 mmol, see J. Chem. Soc., 1954, 3319-3322) in THF (112 mL) at −78° C. was added BuLi (1.15 mL, 1.6 M in hexanes, 1.8 mmol). The reaction was stirred for 5 minutes at -78° C. and a solution of intermediate 370.1 (200 mg, 1.5 mmol) in THF (2 mL) was added dropwise. The mixture was warmed to ambient temperature over 2 h. Ammonium chloride (80 mg) was added to the mixture and it was concentrated. Purification of the crude material afforded 350 mg of intermediate 370.2 as a white solid. LCMS 294.2 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07576098B2 |
|---|
| 出典データセット | uspto-grants-2009_08 |
|---|
| ORD ID | ord-5c8093b6e5674cf79276a67fecbf85d8 |
|---|
| 出典メモ | uspto-grants-2009_08 |
|---|