関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Benzene, 1,3-dichloro-2-iodo-5-nitro- | HCID 112948 | — |
| 反応物 | 4-Fluoro-3-methylphenol | HCID 2737394 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 3,5-Dichloro-4-(4-fluoro-3-methyl-phenoxy)-nitrobenzene | HCID 18614274 | 82.9% |
反応手順
A mixture of 3-methyl-4-fluorophenol (99 mg, 0.79 mmol), potassium hydroxide (53 mg, 0.94 mmol), 4-iodo-3,5-dichloro-nitrobenzene (250 mg, 0.79 mmol) and 4A° molecular sieves (75 mg) in N-methylpyrolidinone (3 mL) was stirred at 130° C. for 2 h. The reaction mixture was poured into ice cold 1 N HCl (20 mL) and EtOAc (25 mL) was added. The EtOAc phase was separated and washed with 1N HCl (3×25 mL) and brine (25 mL). The EtOAc solution was dried over Na2SO4, filtered and concentrated. The residue was purified by preparative TLC (Hexanes: CH2Cl2=7:3) to afford 3,5-dichloro-4-(4-fluoro-3-methyl-phenoxy)-nitrobenzene (207 mg). MS Calc.: 315.0 Found: 315.0 (M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06545018B2 |
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| 出典データセット | uspto-grants-2003_04 |
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| ORD ID | ord-963df51208f8457fab8547ffcd02c8cb |
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| 出典メモ | uspto-grants-2003_04 |
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