Sodium Methoxide → 2-Chloro-7,8-dihydro-1,6-naphthyridin-5(6H)-one
반응식
COC([N:5]1[CH2:14][CH2:13][C:12]2[N:11]=[C:10]([Cl:15])[CH:9]=[CH:8][C:7]=2[C:6]1=[O:16])=O.C[O-].[Na+]>O1CCOCC1>[Cl:15][C:10]1[CH:9]=[CH:8][C:7]2[C:6](=[O:16])[NH:5][CH2:14][CH2:13][C:12]=2[N:11]=1참가 물질
4
실험 절차
A mixture of 2-chloro-5-oxo-7,8-dihydro-5H-[1,6]naphthyridine-6-carboxylic acid methyl ester (60 mg, 0.25 mmol) and sodium methoxide (40 mg, 0.75 mmol) in 2 mL of 1,4-dioxane was subject to microwave reaction at 110° C. for 30 min. After removal of 1,4-dioxane, the residue was dissolved in DCM and the DCM solution was washed with water and brine. The organic layer was then dried over anhy. Na2SO4, filtered and concentrated in vacuo to give a crude product. Prep-TLC separation (30% EtOAc in hexane) then afforded the tile compound (28 mg, 63%) as a white solid. MS: 183.1 (M+H+).
후처리
- customreaction at 110° C. for 30 min
- customAfter removal of 1,4-dioxane
- dissolutionthe residue was dissolved in DCM
- washthe DCM solution was washed with water and brine
- customThe organic layer was then dried over anhy
- filtrationNa2SO4, filtered
- concentrationconcentrated in vacuo
- customto give a crude product
- customPrep-TLC separation (30% EtOAc in hexane)
출처 및 근거
- ORD 기록
- ord-5cf99a5986bf47bcb6985c84daa9dee6
- 출처 데이터셋
- uspto-grants-2015_09
- 특허 번호
- US09133158B2
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