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Chlorotrimethylgermane → 2-(4-Trimethylgermylphenyl)-2-methyl-1,3-dioxolane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorotrimethylgermane | HCID 73723 | — |
| 反応物 | 2-(4-Bromophenyl)-2-methyl-1,3-dioxolane | HCID 614920 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Trimethylgermylphenyl)-2-methyl-1,3-dioxolane | HCID 14605651 | 46.6% |
反応手順
To a mixture of 108 mg (4.44 mmol) of magnesium and 766 mg (5.00 mmol) of trimethylgermyl chloride was added a solution of 972 mg (4.00 mmol) of 2-(4-bromophenyl)-2-methyl-1,3-dioxolane in 12 ml of dry tetrahydrofuran (THF) at 40° C. with stirring. The mixture was refluxed for 1.5 hours and stirred at room temperature overnight. An insoluble substance was filtered off and washed with ether. The filtrate and washings were mixed and evaporated. The residue was purified by column chromatography on silica gel [eluent: petroleum ether-methylene chloride (2:1-1:2)] and recrystallized from petroleum ether to give 524 mg of white prisms, m.p. 63.5°-65° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE036477 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-52d40f97a4844656a56177e0f4835b00 |
| 出典メモ | uspto-grants-1999_12 |