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Triethylamine → Benzyl 4-(2-(4-methoxyphenylthio)ethylcarbamoyl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | Benzyl piperidine-1-carboxylate | HCID 228749 | — |
| 反応物 | Ethanamine, 2-[(4-methoxyphenyl)thio]- | HCID 12261932 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Benzyl 4-(2-(4-methoxyphenylthio)ethylcarbamoyl)piperazine-1-carboxylate | HCID 68626717 | — |
反応手順
To a solution of compound 1 (183 mg) in CH2Cl2 (10 mL) was added triphosgene (0.7 eq.) and triethylamine (1.0 eq.) at 0° C. The reaction mixture was stirred for 1 h. at r.t., and N-Cbz-piperidine (1.5 eq.) and Et3N (0.5 mL) were added. The reaction mixture was stirred overnight and washed with 1N HCl and sat NaHCO3 (3×5 mL). The solvents were removed by evaporation under reduced pressure to give the title product 18, which was purified by chromatography (SiO2, CH2Cl2/EtOAc 10:1). Yield: 360 mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618282B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-44b55b8362cc4f0b951d1671d0c489a8 |
| 出典メモ | uspto-grants-2013_12 |