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1,2-Dichloroethane → Ethyl 1-({[(tert-butoxycarbonyl)amino][3-(trifluoromethyl)phenyl]acetyl}amino)cyclopropanecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Ethyl 1-aminocyclopropanecarboxylate | HCID 386204 | — |
| 反応物 | 2-{[(Tert-butoxy)carbonyl]amino}-2-[3-(trifluoromethyl)phenyl]acetic acid | HCID 22309176 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 1-({[(tert-butoxycarbonyl)amino][3-(trifluoromethyl)phenyl]acetyl}amino)cyclopropanecarboxylate | HCID 66801809 | — |
反応手順
A mixture of 500 mg (1.57 mmol) of [(tert-butoxycarbonyl)amino][3-(trifluoromethyl)-phenyl]acetic acid, 243 mg (1.88 mmol) of ethyl 1-aminocyclopropanecarboxylate, 450 mg (2.35 mmol) of EDC and 317 mg (2.35 mmol) of HOBt in 10 ml of DMF was stirred at RT overnight. The reaction mixture was diluted with ethyl acetate and washed twice with 1N hydrochloric acid and once with a saturated aqueous sodium bicarbonate solution. The organic phase was dried over sodium sulphate and then freed from the solvent on a rotary evaporator. The residue was dried under high vacuum. This gave 650 mg (96% of theory) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09034855B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-bdcae72e96dc4e69890096b6d291c9c9 |
| 出典メモ | uspto-grants-2015_05 |