참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chlorotrimethylgermane | HCID 73723 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 반응물 | 2-(3,5-Dibromophenyl)-2-methyl-1,3-dioxolane | HCID 12884905 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(3,5-Bis(trimethylgermyl)phenyl]-2-methyl-1,3-dioxolane | HCID 12884908 | 65% |
| 생성물 | 2-(3-Trimethylgermylphenyl)-2-methyl-1,3-dioxolane | HCID 14605654 | 11% |
반응 단계
To a suspension of 108 mg (4.44 mmol) of magnesium and 765 mg (5.00 mmol) of trimethylgermyl chloride was added a solution of 644 mg (2.00 mmol) of 2-(3,5-dibromophenyl)-2-methyl-1,3-dioxolane in 10 ml of tetrahydrofuran at 40° C., stirred in an atmosphere of argon. The mixture was stirred at 70° C. for 4.5 hr. and at room temperature overnight. The reaction mixture was poured into ice-aqueous sodium bicarbonate solution and extracted with methylene chloride. The solvent was removed to give pale brown crystals, which were purified by column chromatography on silica gel [eluent: methylene chloride-n-hexane (1:1)] to give 514 mg (yield 65%) of 2-[3,5-bis(trimethylgermyl)phenyl]-2-methyl-1,3-dioxolane, m.p. 54° C., and 61 mg (yield 11%) of 2-(3-trimethylgermylphenyl)-2-methyl-1,3-dioxolane and 75 mg of the mixture, in which the ratio was 3:2 (by NMR).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05155249 |
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| 출처 데이터셋 | uspto-grants-1992_10 |
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| ORD ID | ord-41bd66200ed74803aac1e8f5d1700a2a |
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| 출처 메모 | uspto-grants-1992_10 |
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