참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Benzyl chloroformate | HCID 10387 | — |
| 반응물 | Dibenzyl-(2,4-difluoro-phenyl)-amine | HCID 58086650 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Dibenzylamino-2,6-difluoro-benzoic acid benzyl ester | HCID 58477118 | — |
반응 단계
To a solution of dibenzyl-(2,4-difluoro-phenyl)-amine (17.5 g, 0.056 mol) in THF (140 mL), under nitrogen atmosphere, cooled at −78° C., n-butyllithium (1.6 M in hexane, 38 mL, 0.06 mol) was slowly added. The reaction was stirred for 1 hour, and then quickly added via a cannula to a solution of benzyl chloroformate (11.78 mL, 0.084 mol) in THF (140 mL) previously cooled at −78° C. The reaction was then allowed to warm to room temperature, poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 5% ethyl acetate in hexane grading to 10% acetate (quant.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08946250B2 |
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| 출처 데이터셋 | uspto-grants-2015_02 |
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| ORD ID | ord-daf81abe12e84d59b9fffa28da969bab |
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| 출처 메모 | uspto-grants-2015_02 |
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