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N-(tert-Butoxycarbonyl)-1,2-phenylenediamine → tert-Butyl 2-(6-chloronicotinamido)phenylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-(tert-Butoxycarbonyl)-1,2-phenylenediamine | HCID 676311 | — |
| 反応物 | 6-Chloronicotinoyl Chloride | HCID 2782165 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-Butyl 2-(6-chloronicotinamido)phenylcarbamate | HCID 57717462 | — |
反応手順
To a solution of t-butyl (2-aminophenyl)carbamate A1 (10 g, 48.0 mmol) in CH2Cl2 (200 mL) was added 6-chloronicotinoyl chloride (8.5 g, 48.0 mmol). The reaction mixture was concentrated after 2 hours of stirring at room temperature and purified by flash chromatography (10-75% EtOAc/hexanes) to give the Boc-protected nicotinamide B1 confirmed by MS (ESI+): cal'd [M+Na]+370.1, obs'd 370.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07544695B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-699ff260eaa540d5b6a141cb45d25f16 |
| 出典メモ | uspto-grants-2009_06 |