化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → (S)-2-(6-Methoxynaphthalen-2-yl)propyl carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Trichloroacetyl isocyanate | HCID 76400 | — |
| 反応物 | Naproxol | HCID 3032818 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (S)-2-(6-Methoxynaphthalen-2-yl)propyl carbamate | HCID 67413984 | 57.3% |
反応手順
To (S)-2-(6-methoxy-naphthalen-2-yl)-propan-ol (8.0 g, 37 mmol) in CH2Cl2 (200 mL) at 0° C. under N2 was added trichloroacetyl isocyanate (5.5 mL, 44 mmol). After the mixture was stirred at room temperature for 1 hr, the solvent was concentrated. The residue was treated MeOH (300 mL), water (40 mL) and potassium carbonate (21 g, 0.15 mol) and stirred at RT for 2 hrs to form white precipitate. The precipitate was collected by filtration and dissolved with CH2Cl2. The organic phase was washed with water, dried over MgSO4 and concentrated to give 5.5 g of white precipitate (57%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08269043B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-9efa516740a84480af5b5399c4c9b9c7 |
| 出典メモ | uspto-grants-2012_09 |