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Water → 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 反応物 | 2-Methoxymethylphenylhydrazine | HCID 12979365 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole | HCID 11573215 | 46.2% |
反応手順
Into a reactor were fed 6.2 g (31.6 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone, 4.8 g (31.5 m moles) of 2-methoxymethylphenylhydrazine, 4.76 g (34.9 m moles) of zinc chloride and 60 ml of toluene. Refluxing was made for 2 hours with heating. After the completion of the reaction, the reaction mixture was cooled to room temperature. Water and ethyl acetate were added and phase separation was made. The ethyl acetate layer was concentrated. The resulting crystals were washed with diisopropyl ether to obtain 4.57 g (14.6 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole. Yield: 46%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07531654B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-9cf255d73db140c78ebbe8553dcd104d |
| 出典メモ | uspto-grants-2009_05 |