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Diisopropylethylamine → HCID 86714425、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | isoxazol-5-yl-acetic acid | HCID 13042084 | — |
| 反応物 | Methyl 3-amino-4-(pentan-3-ylamino)benzoate | HCID 61311526 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86714425 | HCID 86714425 | 55% |
反応手順
To a solution of 0.71 g of Isoxazol-5-yl-acetic acid in 15 ml of dry DMF 0.38 g of HOAT, 1.29 g of EDC and 3 ml of DIPEA were added at 0° C. After 30 min 1.32 g of 3-amino-4-(1-ethyl-propylamino)-benzoic acid methyl ester were added and the reaction was stirred at it for 16 h. The reaction was then poured into water and extracted with ethyl acetate three times. The combined organic phases were washed with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and concentrated. The crude product was purified by precipitation from diisoprpylether to yield 1.06 g (55%) of 4-(1-Ethyl-propylamino)-3-(2-isoxazol-5-yl-acetylamino)-benzoic acid methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09156796B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-4f8d2823a07a477a86bd754f8de1385b |
| 出典メモ | uspto-grants-2015_10 |