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Water → HCID 53946910、化合物

HRID 343816
ノート
印刷プレビュー

反応式

HRID 343816 の反応式
[Cl:1][C:2]1[C:3]([N:17]([CH2:22][CH2:23][CH2:24][OH:25])[S:18]([CH3:21])(=[O:20])=[O:19])=[C:4]2[C:9](=[CH:10][C:11]=1[CH3:12])[N:8]=[C:7]([O:13][CH3:14])[C:6]([O:15][CH3:16])=[N:5]2.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:27].[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1.O>CN(C=O)C>[C:24]([CH2:23][CH2:22][N:17]([C:3]1[C:2]([Cl:1])=[C:11]([CH3:12])[CH:10]=[C:9]2[C:4]=1[N:5]=[C:6]([O:15][CH3:16])[C:7]([O:13][CH3:14])=[N:8]2)[S:18]([CH3:21])(=[O:20])=[O:19])([OH:27])=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 2724130Cornforth reagentHCID 54567779HCID 54567779、化合物

生成物 1

HCID 53946910HCID 53946910、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-(6-Chloro-7-methyl-2,3-dimethoxyquinoxalin-5-yl)-N-(3-hydroxypropyl)methanesulphonamide (0.94 g, 2.41 mmol) and pyridinium dichromate (2.42 g, 9.63 mmol) in DMF (24 ml) were stirred at room temperature for 18 hours. The reaction mixture was poured into water (25 ml) and extracted twice with dichloromethane. The combined dichloromethane extracts were extracted twice with 10% potassium carbonate solution. The potassium carbonate extracts were acidified to pH1 with 2M HCl and extracted twice with dichloromethane. These combined dichloromethane extracts were dried (MgSO4) and concentrated under reduced pressure to give N-(2-carboxyethyl)-N-(6-chloro-7-methyl-2,3-dimethoxyquinoxalin-5-yl)methanesulphonamide an off-white solid (0.49 g, 51%).

後処理

  1. extractionextracted twice with dichloromethane
  2. extractionThe combined dichloromethane extracts were extracted twice with 10% potassium carbonate solution
  3. extractionextracted twice with dichloromethane
  4. dry with materialThese combined dichloromethane extracts were dried (MgSO4)
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d12a0de0ae35476fbd49f20b520330e1
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05863917

反応ノート

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