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Triethylene glycol monomethyl ether → 4-(2-(2-(2-Methoxyethoxy)ethoxy)ethoxy)phthalonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylene glycol monomethyl ether | HCID 8178 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(2-(2-(2-Methoxyethoxy)ethoxy)ethoxy)phthalonitrile | HCID 19065531 | 45% |
反応手順
A mixture of 4-nitrophthalonitrile (1.73 g, 10 mmol), triethylene glycol monomethyl ether (1.52 g, 10 mmol) and dried potassium carbonate (2.76 g, 20 mmol) in anhydrous DMF (15 mL) was stirred overnight at ambient temperature under argon. The solvents were removed in vacuo, and the crude product was purified by column chromatography on silica gel using dichloromethane/methanol mixture (97:3) as an eluent to give the product in 45% yield. [1H NMR (δ, ppm, CDCl3): 7.70 (d, 1H, J=8.7 Hz), 7.31 (d, 1H, J=2.5 Hz), 7.23 (dd, 1H, J=8.7 Hz, J=2.5 Hz), 4.22 (m, 2H), 3.88 (m, 2H), 3.6-3.75 (m, 6H), 3.53 (m, 2H), 3.37 (s, 3H).]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524891B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-128614155516453eb32cc2eb5f74fba1 |
| 出典メモ | uspto-grants-2013_09 |