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Water → 2-t-butyl-4-chloro-5-[{6-(2,2,3,3-tetrafluoropropyloxy)-3-pyridyl}-methylthio]-3(2H)-pyridazinone

HRID 1904255
ノート
印刷プレビュー

反応式

HRID 1904255 の反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([SH:13])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].Cl[CH2:15][C:16]1[CH:17]=[CH:18][C:19]([O:22][CH2:23][C:24]([F:29])([F:28])[CH:25]([F:27])[F:26])=[N:20][CH:21]=1.C(=O)([O-])[O-].[K+].[K+].O>C(#N)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([S:13][CH2:15][C:16]2[CH:21]=[N:20][C:19]([O:22][CH2:23][C:24]([F:29])([F:28])[CH:25]([F:27])[F:26])=[CH:18][CH:17]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:2])[CH3:3]
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 11430Potassium CarbonateHCID 134692424-Chloro-2-(1,1-dimethylethyl)-5-mercapto-3(2H)-pyridazinoneHCID 146718285-Chloromethyl-2-(2,2,3,3-tetrafluoropropyloxy)-pyridine

生成物 1

HCID 146718292-t-butyl-4-chloro-5-[{6-(2,2,3,3-tetrafluoropropyloxy)-3-pyridyl}-methylthio]-3(2H)-pyridazinone収率 90.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In 40 ml of acetonitrile were dissolved 2.2 g of 2-t-butyl-4-chloro-5-mercapto-3(2H)-pyridazinone and 2.7 g of 5-chloromethyl-2-(2,2,3,3-tetrafluoropropyloxy)-pyridine, and thereto was added 1.5 g of potassium carbonate. The reaction mixture was stirred overnight at room temperature, poured into water and extracted with benzene. The organic layer was washed with a 5% aqueous solution of sodium hydroxide and then with water, and dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure and the resulting crystals were washed with n-hexane to obtain 4.0 g of 2-t-butyl-4-chloro-5-[{6-(2,2,3,3-tetrafluoropropyloxy)-3-pyridyl}-methylthio]-3(2H)-pyridazinone, m.p. 113.0°~114.0° C.

後処理

  1. extractionextracted with benzene
  2. washThe organic layer was washed with a 5% aqueous solution of sodium hydroxide
  3. dry with materialwith water, and dried over anhydrous sodium sulfate
  4. distillationSolvent was distilled off under reduced pressure
  5. washthe resulting crystals were washed with n-hexane

出典と根拠

ORDレコード
ord-ec069042ebfe4ee58791184e9f2db47b
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04837217

反応ノート

読み込み中…

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