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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

반응식

참여 물질

역할이름HCID투입량
반응물Potassium CarbonateHCID 11430—
반응물5-Bromo-2,2-difluoro-1,3-benzodioxoleHCID 2736271—
반응물1,4-Dioxa-10-azadispiro[4.2.4.2]tetradecan-9-oneHCID 58230108—
용매TolueneHCID 1140—
생성물10-(2,2-Difluoro-benzo[1,3]dioxol-5-yl)-1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-oneHCID 6658042176.8%

반응 조건

온도110 °C

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

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08440710B2
출처 데이터셋uspto-grants-2013_05
ORD IDord-816863bf2a7e4d4ab551257b6d89a0ca
출처 메모uspto-grants-2013_05