関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | N-Methylaniline | HCID 7515 | — |
| 反応物 | Chloro-p-xylene | HCID 32883 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N,2,5-trimethyl-N-phenylaniline | HCID 11042050 | 95% |
反応手順
An oven-dried test tube was purged with argon and charged with Pd2(dba)3 (4.6 mg, 0.005 mmol, 1.0 mol % Pd), 2 [Example 1] (6.0 mg, 0.015 mmol, 1.5 mol %), and NaOt-Bu (135 mg, 1.40 mmol). The test tube was fitted with a septum, then toluene (2.0 mL), N-methylaniline (135 μL, 1.25 mmol), and 2-chloro-p-xylene (135 μL, 1.01 mmol) were added. The mixture was stirred at 80° C. for 13 h, then cooled to room temperature, diluted with ether (20 mL), filtered and concentrated. The crude material was purified by flash chromatography on silica gel to afford 202 mg (95%) of a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06307087B1 |
|---|
| 出典データセット | uspto-grants-2001_10 |
|---|
| ORD ID | ord-abe61cf2f5174f308cab0c3eb5ed35e5 |
|---|
| 出典メモ | uspto-grants-2001_10 |
|---|
