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Water → 6-(1-chloro-2-oxo-2-phenylethyl)-2-isopropyl-3(2H)-pyridazinone

HRID 915012
ノート
印刷プレビュー

反応式

HRID 915012 の反応式
[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([CH2:11][C:12](=[O:19])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:5]1)([CH3:3])[CH3:2].S(Cl)([Cl:23])(=O)=O.O.CCOC(C)=O>C(Cl)Cl>[Cl:23][CH:11]([C:6]1[CH:7]=[CH:8][C:9](=[O:10])[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=1)[C:12](=[O:19])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 24648Sulfuryl chlorideHCID 693314642-isopropyl-6-(2-oxo-2-phenylethyl)-3(2H)-pyridazinone

生成物 1

HCID 858295066-(1-chloro-2-oxo-2-phenylethyl)-2-isopropyl-3(2H)-pyridazinone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2-isopropyl-6-(2-oxo-2-phenylethyl)-3(2H)-pyridazinone (100 g) and sulfurylchloride (32.9 ml) in CH2Cl2 (200 ml) was refluxed with stirring for 5 hours. Water and EtOAc were added to the reaction mixture. The organic layer was separated, and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluted with a mixture of n-hexane and EtOAc. The fractions were concentrated in vacuo to obtain 6-(1-chloro-2-oxo-2-phenylethyl)-2-isopropyl-3(2H)-pyridazinone (100 g) as white powder.

後処理

  1. temperaturewas refluxed
  2. customThe organic layer was separated
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed in vacuo
  5. customThe residue was purified by silica gel column chromatography
  6. washeluted with a mixture of n-hexane and EtOAc
  7. concentrationThe fractions were concentrated in vacuo

出典と根拠

ORDレコード
ord-1148ceb74662448d84e3c15ad4dca89d
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265120B2

反応ノート

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