関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 2-Fluoroanisole | HCID 67576 | — |
| 反応物 | 11-Acetamidoundecanoic acid | HCID 454085 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 11-Acetylamino-undecanoyl chloride | HCID 18434292 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[11-(3-fluoro-4-methoxy-phenyl)-11-oxo-undecyl]acetamide | HCID 18434110 | 107.7% |
反応手順
0.5 ml of oxalyl chloride is added to a solution of 1.2 g of 11-acetylamino-undecanoic acid and 5 drops of DMF in 15 ml of methylene chloride at 0° C. and the mixture is stirred at RT for 3 hrs. The solution of the 11-acetylamino-undecanoyl chloride is treated under argon with 0.6 g of 2-fluoroanisole, cooled to -15° C. and treated with 1.4 g of aluminium chloride. After 2 hrs. at -15° C. the mixture is left to warm to room temperature overnight. The solution is treated with 15 ml of 1 M hydrochloric acid at 0° C. and then with 20 ml of water. The organic phase is separated and washed with 1M hydrochloric acid, with water and with saturated sodium bicarbonate solution, dried and concentrated. 1.8 g of N-[11-(3-fluoro-4-methoxy-phenyl)-11-oxo-undecyl]acetamide are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06034275 |
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| 出典データセット | uspto-grants-2000_03 |
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| ORD ID | ord-8675035257cf471d9f9724dc9537f811 |
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| 出典メモ | uspto-grants-2000_03 |
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