関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile | HCID 13630721 | — |
| 生成物 | 2-(2,4-Dichloro-5-fluorobenzoyl)3-methoxy-acrylonitrile | HCID 53732547 | 99% |
反応手順
A mixture of 21 g of 2,4-dichloro-5-fluorobenzoyl-acetonitrile, 19.2 g of methyl o-formate and 23.1 g of acetic anhydride is refluxed at a bath temperature of 150° C. for 3 hours. The volatile constituents are then distilled off under a waterpump vacuum and finally under a fine vacuum at a bath temperature of 120° C. 24.5 g (99%) of 2-(2,4-dichloro-5-fluorobenzoyl)-3-methoxy-acrylonitrile are obtained. A sample recrystallized from toluene gives colorless crystals of melting point 159° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04914228 |
|---|
| 出典データセット | uspto-grants-1990_04 |
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| ORD ID | ord-0d399a20e9cd45329292df7dbba4f7d2 |
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| 出典メモ | uspto-grants-1990_04 |
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