関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Acrylonitrile | HCID 7855 | — |
| 反応物 | 2-(N-Methylanilino)ethanol | HCID 62340 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Cyanoethoxyethylmethylaniline | HCID 54230077 | — |
反応手順
In a one-gallon autoclave was charged 1019 gm (6.75 moles) of hydroxyethylmethylaniline, 3 gm of anhydrous lithium hydroxide, and 532 gm (10 moles) of acrylonitrile. The autoclave was sealed and slowly heated to 50° C. until the initial exotherm was over. The reaction was then heated to 65°-70° C. for 6 hours. The reaction contents were cooled to room temperature and made slightly acidic with acetic acid. The reaction contents were then filtered. The crude filtered reaction product was stripped of all excess acrylonitrile under vacuum (15-30 mm Hg) at a temperature not exceeding 80° C. to give the orange liquid, 2-cyanoethoxyethylmethylaniline. Liquid chromatography showed the product to be about 97.4% purity. The IR, NMR, and GC mass spectra of the product were consistent with 2-cyanoethoxyethylmethylaniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04381265 |
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| 出典データセット | uspto-grants-1983_04 |
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| ORD ID | ord-4e6004a95ea4413c926852d1deb39623 |
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| 出典メモ | uspto-grants-1983_04 |
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