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Dimethylformamide → 4-(1-Ethyl-propylamino)-6-methyl-2-(2,4,6-trimethyl-phenylamino)-nicotinic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N,N,2-Trimethylaniline | HCID 11869 | — |
| 反応物 | 2-Chloro-4-(1-ethyl-propylamino)-6-methyl-nicotinic acid methyl ester | HCID 24806876 | — |
| 触媒 | Copper | HCID 23978 | — |
| 生成物 | 4-(1-Ethyl-propylamino)-6-methyl-2-(2,4,6-trimethyl-phenylamino)-nicotinic acid methyl ester | HCID 69587262 | — |
反応手順
A mixture of 2-chloro-4-(1-ethyl-propylamino)-6-methyl-nicotinic acid methyl ester, trimethylaniline, potassium carbonate, copper in DMF was heated at reflux. The mixture was quenched with ammonium chloride and stirred for 20 min, filtered through celite and washed with ethyl acetate. The filtrate was extracted with ethyl acetate. The organic layer was separated, dried and concentrated to dryness. The residue was purified through silica gel column chromatography using 2% methanol in chloroform as eluent to give the title compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07125880B1 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-4f03e17beaa84580b5c35b5b6b64d128 |
| 出典メモ | uspto-grants-2006_10 |