참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tributylstannane | HCID 5948 | — |
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | 4-Benzyloxybenzyl chloride | HCID 70042 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (4-Benzyloxy-benzyl)-tributyl-stannane | HCID 59255482 | 83% |
반응 단계
To a mixture of diisopropylamine (1.1 mL, 7.7 mmol) and tetrahydrofuran (20 mL) was added dropwise n-butyl lithium (1.6 M n-hexane solution, 4.5 mL, 7.1 mmol) at −78° C., which was stirred for 30 minutes at that temperature. Tributyltin hydride (1.7 mL, 6.5 mmol) was added dropwise to the reaction mixture at the same temperature and then stirred for 30 minutes at 0° C. The reaction mixture was cooled to −78° C., and a mixture of 4-benzyloxybenzyl chloride (1.5 g, 6.5 mmol) and tetrahydrofuran (10 mL) was added dropwise at that temperature. The reaction mixture was gradually warmed to room temperature. The reaction mixture was partitioned into water and n-heptane. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:30) to obtain the title compound (2.6 g, 83%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841327B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-31b3db9e6cf14de993de3e9ef9c110f5 |
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| 출처 메모 | uspto-grants-2014_09 |
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