Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 2092705생성일: 2026년 10월 26일
Potassium Carbonate → 10-(2,2-Difluoro-benzo[1,3]dioxol-5-yl)-1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-one
https://huagongshe.com/reaction/2092705
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 5-Bromo-2,2-difluoro-1,3-benzodioxole | HCID 2736271 | — |
| 반응물 | 1,4-Dioxa-10-azadispiro[4.2.4.2]tetradecan-9-one | HCID 58230108 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 10-(2,2-Difluoro-benzo[1,3]dioxol-5-yl)-1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-one | HCID 66580421 | 76.8% |
반응 단계
To a mixture of 1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-one (262 mg, 1.24 mmol, obtained in example 133, step 3), potassium carbonate (790 mg, 3.72 mmol) and cuprous iodide (354 mg, 1.86 mmol) was added a solution of 5-bromo-2,2-difluoro-benzo[1,3]dioxole (588 mg, 2.48 mmol) in 5 ml toluene under argon. The solution was then degassed by bubbling argon through the mixture for 2 mins after which N—N′-dimethylethylenediamine (266 uL, 2.48 mmol) was added. The sealed tube was closed and the mixture was heated to 110° C. overnight. The reaction mixture was then cooled to room temperature and filtered through a short pad of Celite® using ethyl acetate to wash the mixture through. The solution was then concentrated in vacuo to give a residue which was purified by flash column chromatography (3:7 ethyl acetate heptane) to give the title compound as white solid (350 mg, 75%). MS (m/e): 368.0 [MH+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08440710B2 |
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| 출처 데이터셋 | uspto-grants-2013_05 |
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| ORD ID | ord-816863bf2a7e4d4ab551257b6d89a0ca |
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| 출처 메모 | uspto-grants-2013_05 |
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