関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Bis(2-chloroethyl) ether | HCID 8115 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | tert-butyl N-(3-aminophenyl)carbamate | HCID 12877220 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Tert-butyl (3-morpholinophenyl)carbamate | HCID 101043125 | 58.3% |
反応手順
To a suspension of tert-butyl (3-aminophenyl)carbamate (7.59 g, 36.40 mmol), K2CO3 (10.06 g, 72.80 mmol) and NaI (16.37 g, 109.20 mmol) in DMF (300 mL) was added 2,2′-dichlorodiethyl ether (5.73 g, 40.1 mmol) slowly at 150° C. under N2. The reaction mixture was stirred at 150° C. overnight, then cooled to rt, poured into water (700 mL) and extracted with CH2Cl2 (200 mL×3). The combined organic phases were washed with water (200 mL×3) and brine (200 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1) to give the title compound as a yellow solid (5.91 g, 58%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434695B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-02c84d3d9b0546dbbe946147c6594b9c |
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| 出典メモ | uspto-grants-2016_09 |
|---|
