関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 反応物 | 4-Heptanamine | HCID 38665 | — |
| 反応物 | 3-(2,6-Dichlorophenyl)-3-oxopropiononitrile | HCID 3018140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (E)-2-(2,6-dichlorobenzoyl)-3-(1-propylbutylamino)acrylonitrile | HCID 67267339 | 10.5% |
反応手順
A mixture of 3-(2,6-dichlorophenyl)-3-oxopropanenitrile (0.200 g, 0.93 mmol), acetic anhydride (0.22 g, 2.20 mmol), and triethyl orthoformate (0.21 g, 1.40 mmol) was stirred at 150° C. for 1 hr. The solution was then concentrated and the residue redissolved in ethanol (5 mL). 4-heptylamine (0.16 g, 1.4 mmol) in 1 mL of tetrahydrofuran was added to the reaction mixture at 0° C. The reaction stirred for 30 minutes and was then concentrated. Flash chromatography (20% Ethyl acetate/hexanes) gave the desired compound (0.033 g, 10%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07897607B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-c02c2c1bc69342f3afc648452bc0ea63 |
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| 出典メモ | uspto-grants-2011_03 |
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