Sodium Chloride → 1-(2-(1-hydroxy-4-oxocyclohexyl)ethyl)-7-methoxyquinoxalin-2(1H)-one

HRID 39750ノート

反応式

HRID 39750 の反応式
[OH:1][C:2]1([CH2:12][CH2:13][N:14]2[C:23]3[C:18](=[CH:19][CH:20]=[C:21]([O:24][CH3:25])[CH:22]=3)[N:17]=[CH:16][C:15]2=[O:26])[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4][CH2:3]1.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+].[Cl-].[Na+]>C(OCC)(=O)C.O1CCOCC1>[OH:1][C:2]1([CH2:12][CH2:13][N:14]2[C:23]3[C:18](=[CH:19][CH:20]=[C:21]([O:24][CH3:25])[CH:22]=3)[N:17]=[CH:16][C:15]2=[O:26])[CH2:11][CH2:10][C:5](=[O:6])[CH2:4][CH2:3]1

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 593979861-(2-(8-Hydroxy-1,4-dioxaspiro(4.5)decan-8-yl)ethyl)-7-methoxyquinoxalin-2(1h)-one

生成物 1

HCID 593979991-(2-(1-hydroxy-4-oxocyclohexyl)ethyl)-7-methoxyquinoxalin-2(1H)-one

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

To 8 mL of a dioxane suspension containing 0.25 g of 1-(2-(8-hydroxy-1,4-dioxaspiro(4.5)decan-8-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one, 3 mL of an 80% aqueous trifluoroacetic acid solution was dividedly added at room temperature, and the mixture was stirred for 5 hours and 15 minutes. An aqueous saturated sodium hydrogen carbonate solution was added with the reaction mixture, and then added with ethyl acetate and sodium chloride. The organic layer was separated, and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent; hexane:ethyl acetate 1:3] to obtain 0.10 g of a colorless oily substance, 1-(2-(1-hydroxy-4-oxocyclohexyl)ethyl)-7-methoxyquinoxalin-2(1H)-one.

後処理

  1. additionwas dividedly added at room temperature
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe residue thus obtained
  6. customwas purified by silica gel column chromatography [eluent; hexane:ethyl acetate 1:3]

出典と根拠

ORDレコード
ord-8044680539924a2fa98b69bfc676ca83
出典データセット
uspto-grants-2013_09
特許番号
US08524738B2

反応ノート

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