関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(2-Bromo-4-fluoro-phenyl)-butane-1,4-diol | HCID 57445090 | — |
| 触媒 | Platinous chloride | HCID 2770 | — |
| 触媒 | Silver hexafluoroantimonate | HCID 16687962 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 生成物 | 2-(2-Bromo-4-fluoro-phenyl)-tetrahydro-furan | HCID 57445091 | 77.3% |
反応手順
Combine 1-(2-bromo-4-fluoro-phenyl)-butane-1,4-diol (1 g, 3.8 mmol), silver (I)hexafluoroantimonate (131 mg, 0.4 mmol), platinum(II) chloride (40 mg, 0.2 mmol) in 1,2-dichloroethane (10 mL) in a pressure tube. Seal the tube and heat the mixture overnight at 110° C. Dilute the mixture with chloroform-IPA (3:1, 100 mL). Wash the organic phase with aqueous saturated sodium chloride and water. Dry the mixture over sodium sulfate. Concentrate the solution in vacuo. Purify by column chromatography (20% ethyl acetate in hexane) to give the title compound as a pale yellow oil (0.72 g, 77%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08063035B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-95ac991e75c34e8f80fa54d834ab4ec3 |
|---|
| 出典メモ | uspto-grants-2011_11 |
|---|