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Water → 3,4-Dihydro-1H-2-benzopyran-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 生成物 | 3,4-Dihydro-1H-2-benzopyran-1-ol | HCID 13613708 | 95% |
反応手順
To a solution of methyl-3-(2'-formyl-3'-6'-dimethoxy)phenyl-2-methoxyisopropyloxy-propionate (4.2 g, 12.4 mmol) in THF (75 ml) containing water (4 ml) was added pyridinium p-toluenesulfonate (230 mg). After stirring at room temperature for 1.75 hours, triethylamine (3 ml) and saturated NH4Cl solution (60 ml) were added. THF was removed at 25° C. and the mixture was extracted with ether (3×150 ml). Ether extract was washed with brine, dried and evaporated yielding 3.9 g of 1-hydroxyisochroman (95%) (quite pure from NMR spectrum). (MP. 127°-129° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05593970 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-1a91f95f18444534942176066df07556 |
| 出典メモ | uspto-grants-1997_01 |