関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,2-Dibromopropane | HCID 11658 | — |
| 反応物 | 7-Chlorodibenzofuran-3-ol | HCID 20429499 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 1-Bromo-3-(7-chlorodibenzofuran-3-oxy)-propane | HCID 20429506 | 50.4% |
反応手順
A mixture of 98.4 g (0.45 mole) of 7-chlorodibenzofuran-3-ol, 200 ml of methyl ethyl ketone, 93 g (0.67 mole) of potassium carbonate and 283 g (1.4 moles) of dibromopropane was refluxed for 24 hours. The inorganic precipitate was filtered off with suction and the filtrate was concentrated under reduced pressure. The residue was dissolved in 500 ml of methylene chloride and the solution was washed with 100 ml of water, 100 ml of 2 N sodium hydroxide solution and 100 ml of water in succession, dried over sodium sulfate and concentrated under reduced pressure. The solid residue was left to stand with 30 ml of pentane at 0° C. for 30 minutes, filtered off with suction and washed with 30 ml of cold n-pentane. 77 g of pure 1-bromo-3-(7-chlorodibenzofuran-3-oxy)-propane of melting point 83°-85° C. were obtained; yield: 50% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04376776 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-53aae8a75c18456fa8b709f87e828e9f |
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| 出典メモ | uspto-grants-1983_03 |
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