関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | N-Boc-4-hydroxyaniline | HCID 2756771 | — |
| 反応物 | N-(4-fluoro-3-nitrophenyl)benzamide | HCID 3535228 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | [4-(4-Benzoylamino-2-nitrophenoxy)-phenyl]carbamic acid tert-butyl ester | HCID 67040356 | 93.1% |
反応手順
A mixture of N-(4-fluoro-3-nitrophenyl)benzamide (1.00 g, 3.8 mmol), N-Boc-4-hydroxyaniline (0.83 g, 3.8 mmol) and 85% KOH (0.51 g, 7.7 mmol) in DMSO (20 mL) was heated at 80° C. for 1 hour, and then poured into H2O (100 ml) under stirring. The resulting oily crystal was extracted with EtOAc. The extract was washed with H2O (3 times) and brine, dried over MgSO4, filtered and concentrated under vacuum giving the crude title compound, which was purified by washing with i-Pr2O to give the desired compound as yellow crystals (1.59 g, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07910595B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-0346ac4040c94a799838694124054c87 |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|