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2,5-Dichlorobenzoic acid → 3-Chloro-6-(3,5-diisopropylphenoxy)benzoic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dichlorobenzoic acid | HCID 5784 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3,5-Bis(1-methylethyl)phenol | HCID 93104 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 3-Chloro-6-(3,5-diisopropylphenoxy)benzoic Acid | HCID 20298967 | 49.4% |
反応手順
2,5-dichlorobenzoic acid (5 g) and 3,5-diisopropylphenol (4.66 g) were dissolved in dry xylene and the solution placed under dry oxygen-free nitrogen. Sodium hydride (1.25 g) was added as a suspension in petroleum ether. Cuprous bromide was added and the solution refluxed for 5 hours and cooled. The xylene was removed by low pressure distillation. The remaining solid was acidified with dilute hydrochloric acid and extracted with diethyl ether. The ethereal layer was separated, dried and distilled under low pressure to give an oil. The oil was dissolved in petroleum ether (30°-40° ). Standing gave a crystalline solid, which was recrystallised from hexane to give the title compound (4.3 g), mp 129°-130° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04242121 |
| 出典データセット | uspto-grants-1980_12 |
| ORD ID | ord-c41674c889ed47979e95692495323db8 |
| 出典メモ | uspto-grants-1980_12 |