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Cyanic acid → Tetrahydropyranyl ether
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanic acid | HCID 540 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tetrahydropyranyl ether | HCID 263182 | — |
反応手順
A solution of 1.23 g of Part F cyano-alcohol (7.36 mmole) in 20 ml of dry methylene chloride was treated with 800 ml of dihydropyran (8.89 mmole) and catalytic amount of p-toluene sulfonic acid at 0°-5° C. After 4 hours, the reaction mixture was diluted with ether and washed with aqueous sodium bicarbonate solution. The aqueous layer was reextracted twice with ether. The combined organic extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The crude residue was chromatographed on a silica gel column and eluted with 20-25% ethyl acetate in hexane to obtain 1.61 g of title tetrahydropyranyl ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04611006 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-8d26df4c844841088d52bed2ea1d89a7 |
| 出典メモ | uspto-grants-1986_09 |