関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dihexylamine | HCID 8920 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-fluoro-N,N-di-n-hexyl-4-nitroaniline | HCID 90024145 | 86% |
反応手順
To a solution of 3,4-difluoronitrobenzene (1.59 g, 10 mmol) in DMSO (15 mL) were added K2CO3 (3.04 g, 22 mmol) and di-n-hexylamine (2.04 g, 11 mmol). The mixture was heated at 90° C. overnight, then cooled to rt, diluted with water (50 mL) and extracted with CH2Cl2 (50 mL×3). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/CH2Cl2 (V/V)=10:1) to give the title compound as pale yellow oil (2.79 g, 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434695B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-ba52dcdca5224e56bb6328da85a7e25d |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
