참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trityl chloride | HCID 6456 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (2-Bromo-4-hydroxymethylphenyl)methanol | HCID 18676617 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Bromo-1,4-bis(trityloxymethyl)benzene | HCID 68458085 | 18.1% |
반응 단계
Under a nitrogen stream, to a solution of trityl chloride (11.58 g, 41.6 mmol) and (2-bromo-4-hydroxymethylphenyl)methanol (4.1 g, 18.9 mmol) in DMF (12 ml), triethylamine (5.8 ml, 41.6 mmol) and DMAP (369.2 mg, 3.02 mmol) were added and the mixture was stirred for 18 hours at room temperature. The reaction mixture was evaporated under reduced pressure to remove the solvent and then extracted with methylene chloride. The organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and then evaporated under reduced pressure to remove the solvent. The resulting residue was purified by silica gel column chromatography (developing solution=ethyl acetate:n-hexane (1:2)) to give the titled compound (2.4 g, 18%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07767651B2 |
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| 출처 데이터셋 | uspto-grants-2010_08 |
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| ORD ID | ord-8ccba11ff0d24bf381beccbd5c88c6d2 |
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| 출처 메모 | uspto-grants-2010_08 |
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