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 | 2-(Benzyloxy)propan-1-amine | HCID 296015 | — |
| 反応物 | 2-[(Tert-butyldimethylsilyl)oxy]-4-nitroaniline | HCID 15485710 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(2-Hydroxy-4-nitrophenyl)-N'-(2-benzyloxypropyl)urea | HCID 15485714 | 103% |
反応手順
To a solution of 2-tert-butyldimethylsilyloxy-4-nitroaniline (300 mg, 1.125 mmol) in toluene (10 mL), triphosgene (126 mg, 0.45 mmol) and triethylamine (0.195 mL, 1.35 mmol) were added. The reaction mixture was stirred at 80° C. for 3 hours. Then it was cooled to room temperature and all solvent was evaporated. The residue was dissolved in DMF (1 mL) and 2-benzyloxypropylamine (185.6 mg, 1.125 mmol) was added. The reaction mixture was stirred at 80° C. for 16 hours. Chromatography of the resulting liquid on silica gel (50% Ethyl acetate/Hexane) gave desired product (160 mg, 41%). EI-MS m/z 346.4 (M+). mp: 64.6-65.2° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06133319 |
|---|
| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-07e213e56cea42cebb574def8e748fdd |
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| 出典メモ | uspto-grants-2000_10 |
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