関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Calcium Bromide | HCID 5360316 | — |
| 反応物 | Calcium Hydroxide | HCID 6093208 | — |
| 反応物 | alpha-(2,3-Dibromopropyl)-2,4-difluorobenzenemethanol | HCID 18923963 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (+/-)-4-Bromo-2-(2,4-difluorophenyl)tetrahydrofuran | HCID 85719042 | 57% |
反応手順
A mixture of 4.5 g of product from Example 164, 1.67 g of calcium hydroxide, 7.5 g of calcium bromide, 25 ml of water and 12 ml of methyl alcohol is stirred and heated at 85° C. overnight. The reaction mixture is cooled, diluted with ethyl acetate and filtered through diatomaceous earth. The layers are separated and the organic layer is washed with saturated sodium chloride, dried, filtered and concentrated in vacuo. The residue is purified by chromatography (silica gel: 3-5% ethyl acetate/hexane) to give 1.96 g of the desired product as a mixture of isomers.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05623081 |
|---|
| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-346c59c7b65f4ddba6f8c0daab77efe2 |
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| 出典メモ | uspto-grants-1997_04 |
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