関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trichloroisocyanuric Acid | HCID 6909 | — |
| 反応物 | 4-Fluoro-2-nitrotoluene | HCID 67965 | — |
| 反応物 | Acetic acid sulfuric acid | HCID 23350293 | — |
| 生成物 | 4-Methylcatechol | HCID 9958 | 33.1% |
反応手順
TCCA (16.7 g, 72 mmol) was added to a solution of 4-fluoro-1-methyl-2-nitrobenzene (12.4 g, 80 mmol) in CH3CO2H/H2SO4 (80 mL/80 mL). The mixture was heated to 70° C. and stirred overnight. After cooling to room temperature, the reaction mixture was poured into ice water (1000 mL) and extracted with DCM (2×200 mL). The combined organic phase was washed with brine and concentrated in vacuo. The residue was purified by column chromatography (PE: EA=50:1) to give compound 1 (5.0 g, 33.1%) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434724B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-6a5d8e0b4f2f48f6baff74346c1a6d6d |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
