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p-Toluenesulfonic acid → 2-Methoxy-5-((tetrahydro-2H-pyran-2-yl)oxy)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 反応物 | 5-Hydroxy-2-methoxypyridine | HCID 11622335 | — |
| 反応物 | Water methylene chloride | HCID 21908982 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methoxy-5-((tetrahydro-2H-pyran-2-yl)oxy)pyridine | HCID 117622661 | — |
反応手順
10.1 g (119.9 mmol, 1.5 eq.) of 3,4-dihydro-2H-pyran and 1.4 g (8.0 mmol, 0.1 eq.) of 4-toluenesulphonic acid were added to a solution of 10.0 g (79.9 mmol) of 6-methoxypyridin-3-ol in 150 ml of dichloromethane, and the mixture was stirred at RT for 5 d. After addition of water/dichloromethane and phase separation, the aqueous phase was extracted with dichloromethane. The combined organic phases were dried (sodium sulphate), filtered and concentrated under reduced pressure. Yield: 17.3 g (100% of theory)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434690B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-d6770c83df914ad7bc6d1b64050071cf |
| 出典メモ | uspto-grants-2016_09 |