関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitroaniline | HCID 6946 | — |
| 反応物 | 2,4,4-Trimethyl-1-pentene | HCID 7868 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 4-Tert-octyl-2-nitroaniline | HCID 14122178 | — |
反応手順
In a 2-liter reaction flask fitted with a condenser, nitrogen inlet, stirrer, thermometer and addition funnel is placed 272 grams (2.0 moles) of anhydrous zinc chloride. The flask is placed under a nitrogen atmosphere and 166 ml (2.0 moles) of concentrated (12 N) hydrochloric acid is added over a 10-minute period with the temperature rising from 22° to 40° C. To this is then added 276 grams (2.0 moles) of o-nitroaniline over a 15-minute period to avoid the formation of lumps. The resulting thick red slurry is heated to 60° C. and then 474 grams (3.0 moles) of diisobutylene is added gradually over a 110-minute period with the temperature rising during this period from 60° to 90° C. The deep red fluid reaction mixture is heated for another 18 hours at reflux till only a trace of o-nitroaniline is observed by thin layer chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04727158 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-3497fce3c27c4a8183dd59dfdd64c3b5 |
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| 出典メモ | uspto-grants-1988_02 |
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