참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Boron trifluoride etherate | HCID 8000 | — |
| 반응물 | Trifluoroacetic anhydride | HCID 9845 | — |
| 반응물 | 2-(Phenoxymethyl)benzoic acid | HCID 69761 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Dibenz[b,e]oxepin-11(6H)-one | HCID 78259 | 98% |
반응 단계
The 2-(phenoxymethyl)benzoic acid (22.18 g, 97 mmol) was dissolved in DCM (200 mL) and trifluoroacetic anhydride (20.59 mL, 146 mmol) was added, followed by a catalytic amount of borontrifluoride etherate (2.22 mL, 17.5 mmol). The reaction mixture was heated at 40° C. for 2 hours. The solution was then washed with water, sodium bicarbonate (saturated solution) and water. The organic phases was dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product was purified on silica gel (10-20% ethyl acetate in hexanes) to afford title compound 482 (19.937 g, 98%) as a light pink solid. MS (m/z): 211.1 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09193749B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-66b607ca772f4e40bce4652b7021ae2c |
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| 출처 메모 | uspto-grants-2015_11 |
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