Sodium Methoxide → 2-Chloro-7,8-dihydro-1,6-naphthyridin-5(6H)-one
反応式
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]=1参加物
4
実験手順
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+).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-5cf99a5986bf47bcb6985c84daa9dee6
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09133158B2
反応ノート
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