참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cycloheptylamine | HCID 2899 | — |
| 반응물 | Bromoacetyl bromide | HCID 61147 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Bromo-N-(cycloheptyl)acetamide | HCID 22251574 | 89.7% |
반응 단계
To a -20° C. solution of cycloheptylamine (6.37 mL, 50.0 mmol) and diisopropylethylamine (9.58 mL, 55.0 mmol) in methylene chloride (250 mL) was slowly added bromoacetyl bromide (4.78 mL, 55.0 mmol). The reaction mixture was warmed to room temperature over 20 minutes and stirred for an addition 30 minutes. The reaction mixture was diluted with water (100 mL) and stirred for an additional 30 minutes. The organic layer was separated, washed with water (3×100 mL), dried over magnesium sulfate and concentrated in vacuo to afford a beige solid (10.5 g). The crude material was further purified by silica gel flash column chromatography using hexane-ethyl acetate (1:1) as the eluent to give the purified title compound as a white solid (9.77 g, 83%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05817489 |
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| 출처 데이터셋 | uspto-grants-1998_10 |
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| ORD ID | ord-ae64552625364ae89b87637c8606f74d |
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| 출처 메모 | uspto-grants-1998_10 |
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