참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Epichlorohydrin | HCID 7835 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 5-Bromosalicylaldehyde | HCID 72863 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | (7-Bromo-2,3-dihydrobenzo[b][1,4]dioxin-2-yl)methanol | HCID 233965 | 44% |
반응 단계
To a stirred solution of 5-bromosalicylaldehyde (5.0 g, 24.9 mmol), and epichlorohydrin (5.6 mL, 72.1 mmol) in 20 mL of DMF at 80° C. was added K2CO3 slowly in portions. The resulting mixture was then heated at 90° C. for 3 h. Reaction was then stopped, water was added, extracted with diethyl ether. The organic extracts were washed with water, brine, dried over Na2SO4, concentrated in vacuo. The residue was purified on a SiO2 flash column chromatography eluting with 15-30% EtOAc/hexanes to give 2.82 g (44%) of the title compound as colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06867203B2 |
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| 출처 데이터셋 | uspto-grants-2005_03 |
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| ORD ID | ord-1dc99065235e46769bedd783d4257b57 |
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| 출처 메모 | uspto-grants-2005_03 |
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