참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Diethyl chlorophosphate | HCID 13139 | — |
| 반응물 | n-Butyl lithium | HCID 61028 | — |
| 생성물 | Diethyl vinyl phosphate | HCID 573017 | — |
반응 단계
10 ml of N-butyllithium solution (2.1 M solution in hexane) were added dropwise to 50 ml of abs. THF under an argon atmosphere at 0° C. The solution was stirred for 30 minutes at 0° C. and for 15 hours at room temperature, then added to 3.01 ml diethyl chlorophosphonate (20 mmol) at −76° C. and stirred for 1 h at 0° C., then for 16 hours at room temperature. A white solid was filtered off, and the solvent was removed on a rotary evaporator. The slightly yellowish crude product was purified by column chromatography on silica gel (PE:EE=4:1). 2.2 g (60% of th.) of the title compound were obtained as a yellowish liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08999323B2 |
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| 출처 데이터셋 | uspto-grants-2015_04 |
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| ORD ID | ord-b51dc8cbfe264b779b9b095261875fe1 |
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| 출처 메모 | uspto-grants-2015_04 |
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