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Potassium Carbonate → Tert-butyl 3-{4-[3-(acetylamino)phenyl]-1-piperidinyl}propylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | tert-butyl N-(3-bromopropyl)carbamate | HCID 4460490 | — |
| 反応物 | Acetamide, N-[3-(4-piperidinyl)phenyl]- | HCID 22048943 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Tert-butyl 3-{4-[3-(acetylamino)phenyl]-1-piperidinyl}propylcarbamate | HCID 22049023 | 43.1% |
反応手順
A mixture of N-[3-(4-piperidyl)phenyl]acetamide (550 mg, 2.1 mmol), tert-butyl 3-bromopropylcarbamate (550 mg, 2.3 mmol), K2CO3 (1.10 g, 8.9 mmol), diisopropylethyl amine (1.50 mL) and a few crystals of KI in dioxane (20 mL) was heated at reflux temperature for 2 days. The precipitated salts were removed by filtration, the filtrate was concentrated in vacuo and the crude product was chromatographed on silica to give the desired product (340 mg; 43%): ESMS m/e: 376.2 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07199135B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-b7ccb9d402e441a3b0e6c73cee3131b0 |
| 出典メモ | uspto-grants-2007_04 |