関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyltetrahydrofuran | HCID 7301 | — |
| 反応物 | Tri-n-butylphosphonium tetrafluoroborate | HCID 11818592 | — |
| 反応物 | 6-bromo-1H-isochromen-1-one | HCID 21252047 | — |
| 反応物 | HCID 178419777 | HCID 178419777 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(1,3-Dioxolan-2-ylmethyl)isochromen-1-one | HCID 77230659 | — |
反応手順
A mixture of 6-Bromo-1H-isochromen-1-one (980 mg, 4.4 mmol), tributyl phosphonium tetrafluoroborate (25 mg, 0.087 mmol), palladium (II) acetate (9.8 mg, 0.044 mmol) was suspended in DMF (10 ml) then added bromo(1,3-dioxolan-2-ylmethyl)zinc (9.58 ml, 4.79 mmol) and purged with nitrogen. The reaction was heated to 85° C. for 10 hours and then stirred at RT overnight. Methyl tetrahydrofuran was added and the mixture was washed with brine. The organic layer was dried over MgSO4, filtered and evaporated to dryness. The residue was purified thru a 80 g ISCO Redi-sep column and eluted with 0-100% EtOAc/hexane to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08999990B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-0df325619bf04c4688296e944b0714f0 |
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| 出典メモ | uspto-grants-2015_04 |
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