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Water → 6-(4-Formyl-2-methylphenoxy)nicotinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Hydroxy-3-methylbenzaldehyde | HCID 139901 | — |
| 反応物 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(4-Formyl-2-methylphenoxy)nicotinonitrile | HCID 59730245 | 97.1% |
反応手順
Combine 4-hydroxy-3-methyl-benzaldehyde (401 mg, 2.94 mmol), K2CO3 (570 mg, 4.12 mmol) and 6-chloronicotinonitrile (408 mg, 2.94 mmol) in DMF (6 ml), heat at 100° C. After 4 h cool to ambient temperature and pour into water. Extract the aqueous layer with EtOAc. Dry the organic layer over Na2SO4 and eliminate the solvent. Dry under vacuum at 45° C. overnight to get the title compound (680 mg, 97%). 1H-NMR (CDCl3, 400 MHz): 9.99 (s, 1H), 8.43 (d, 1H, J=2.5 Hz), 7.97 (dd, 1H, J=2.5 and 8.8 Hz), 7.84 (bs, 1H), 7.80 (dd, 1H, J=2.5 and 8.8 Hz), 7.22 (d, 1H, J=8.4 Hz), 7.11 (d, 1H, J=8.4 Hz), 2.24 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381719B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-e6711d9e40a94a29adc61f2855fa4077 |
| 出典メモ | uspto-grants-2008_06 |