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Chloral → (2R, 6R)-2-trichloromethyl-5,6-dimethyl-1,3-dioxan-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloral | HCID 6407 | — |
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (3R)-2-methyl-3-hydroxybutanoic acid | HCID 18633016 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2R, 6R)-2-trichloromethyl-5,6-dimethyl-1,3-dioxan-4-one | HCID 57161429 | 83.5% |
反応手順
A mixture of (3R)-2-methyl-3-hydroxybutanoic acid 3.6 g, chloral 8.3 g, pyridinium p-toluenesulfonate (PPTS) 0.7 g and dichloromethane 20 ml was refluxed for 25 hours under a dehydration condition. 40 ml of a saturated aqueous sodium hydrogen carbonate was added thereto and the resulting separated organic phase was dried over anhydrous magnesium sulfate and the solvent was distilled off to obtain 6.3 g of (2R, 6R)-2-trichloromethyl-5,6-dimethyl-1,3-dioxan-4-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411877 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-1b232995cdb4485884eb9ac2fd24a0fa |
| 出典メモ | uspto-grants-1995_05 |