関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2,6-Dimethylphenol | HCID 11335 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2',6'-Dimethylphenoxy)phthalonitrile | HCID 952073 | 87% |
反応手順
A mixture of 4-nitro-phthalonitrile (1 eq), 2,6-dimethylphenol (1.2 eq), K2CO3 (2 eq), and DMF (1 mL/mmol 4-nitro-phthalonitrile) was heated under nitrogen at 60° C. for 3 h with stirring. After cooling to ambient temperature the mixture was poured into water (6 mL/mL DMF) with stirring. The mixture was extracted twice with EtOAc. The combined organic phases were dried over MgSO4 and concentrated in vacuo. The residue was recrystallized from EtOH to give the title compound as a tan solid (yield: 87%); 1H NMR (CDCl3, 200 MHz): δ=7.70 (d, 1H), 7.05 to 7.16 (m, 5H), 2.08 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08759373B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
|---|
| ORD ID | ord-9978a0cb1dd743ffa8a7648d2010ff6b |
|---|
| 出典メモ | uspto-grants-2014_06 |
|---|
