関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dodecane | HCID 8182 | — |
| 反応物 | N-Methylformamide | HCID 31254 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 1-Iodo-3,5-dimethylbenzene | HCID 140924 | — |
| 反応物 | HCID 178454901 | HCID 178454901 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(3,5-dimethylphenyl)-N-methylformamide | HCID 9855564 | 46% |
反応手順
A Schlenk tube was charged with CuI (9.6 mg, 0.050 mmol, 5.0 mol %), di-tert-butylphosphine oxide (16.5 mg, 0.102 mmol), K3PO4 (430 mg, 2.03 mmol), evacuated, backfilled with Ar. 5-Iodo-m-xylene (145 μL, 1.00 mmol), N-methylformamide (72 μL, 1.23 mmol), and toluene (1.0 mL) were added under Ar. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 110° C. for 24 h. The suspension was allowed to reach room temperature. Dodecane (internal GC standard, 230 μL) and ethyl acetate (2 mL) were added. A 0.1 mL sample of the supernatant solution was diluted with ethyl acetate (1 mL) and analyzed by GC to provide a 46% yield of N-(3,5-dimethylphenyl)-N-methylformamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06759554B2 |
|---|
| 出典データセット | uspto-grants-2004_07 |
|---|
| ORD ID | ord-6982a47636594eb9b94c656b6f9f496f |
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| 出典メモ | uspto-grants-2004_07 |
|---|
