Sodium Carbonate → [1-(2-fluoro-2-methylpropyl)-5-oxido-1H-imidazo[4,5-c][1,5]naphthyridin-2-yl]methyl acetate

HRID 81936ノート

反応式

HRID 81936 の反応式
[C:1]([O:4][CH2:5][C:6]1[N:7]([CH2:19][C:20]([F:23])([CH3:22])[CH3:21])[C:8]2[C:17]3[N:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]=[CH:10][C:9]=2[N:18]=1)(=[O:3])[CH3:2].ClC1C=C(C=CC=1)C(OO)=[O:29].C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[C:1]([O:4][CH2:5][C:6]1[N:7]([CH2:19][C:20]([F:23])([CH3:22])[CH3:21])[C:8]2[C:17]3[N:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N+:11]([O-:29])=[CH:10][C:9]=2[N:18]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 68933078HCID 68933078、化合物

生成物 1

HCID 68935317[1-(2-fluoro-2-methylpropyl)-5-oxido-1H-imidazo[4,5-c][1,5]naphthyridin-2-yl]methyl acetate収率 99.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

[1-(2-Fluoro-2-methylpropyl)-1H-imidazo[4,5-c][1,5]naphthyridin-2-yl]methyl acetate (1.59 g, 5.03 mmol) was dissolved in 50 mL of CH2Cl2 and treated with 3-chloroperoxybenzoic acid (1.52 g, 57-86% purity). After stirring for 2 hours, the reaction mixture was treated with 25 mL of CH2Cl2 and 20 mL of 5% Na2CO3 solution and the layers were separated. The organic layer was washed with H2O (20 mL) and brine (20 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure to give 1.67 g of [1-(2-fluoro-2-methylpropyl)-5-oxido-1H-imidazo[4,5-c][1,5]naphthyridin-2-yl]methyl acetate as an off-white solid.

後処理

  1. customthe layers were separated
  2. washThe organic layer was washed with H2O (20 mL) and brine (20 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f6f548510c834bc1a0eba16e98c3f401
出典データセット
uspto-grants-2014_09
特許番号
US08846710B2

反応ノート

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