참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon tetrabromide | HCID 11205 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 2-(2,2-Dimethyl-1,3-dioxan-5-yl)ethanol | HCID 11816011 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1,3-Dioxane, 5-(2-bromoethyl)-2,2-dimethyl- | HCID 178988 | — |
반응 단계
To a solution of compound 32 (84 g, 0.528 mol) in dry DMF (500 mL) was added triphenylphosphine (207 g, 0.79 mol) with vigorous stirring until it becomes a clear solution. The mixture was cooled to 0° C. and added CBr4 (260 g, 0.79 mol) portion wise over a period of 30 min and allowed to stir at RT for 5 h. The reaction mixture was cooled to 0° C., added saturated NaHCO3 solution (200 mL) and extracted with hexane (4×200 mL). The combined organic layer was dried, concentrated under vacuum and the crude title compound (117 g) was used for next reaction without any purification. TLC: Pet. ether/EtOAc, 7:3, Rf=0.6
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08017620B2 |
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| 출처 데이터셋 | uspto-grants-2011_09 |
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| ORD ID | ord-8a9400e2ee204391b432642c46834d37 |
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| 출처 메모 | uspto-grants-2011_09 |
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