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Water → 2-tert.-butyl-4-methyl-5-methylthio-3(2H)-pyridazinone

HRID 2352014
ノート
印刷プレビュー

反応式

HRID 2352014 の反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8]([SH:13])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].CI.[C:16](=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8]([S:13][CH3:16])[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 6328Methyl iodideHCID 10340Sodium CarbonateHCID 138222652-t-butyl-5-mercapto-4-methyl-3(2H)-pyridazinone

生成物 1

HCID 138251612-tert.-butyl-4-methyl-5-methylthio-3(2H)-pyridazinone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The crude product 2.0 g (0.01 mol) of 2-tert.-butyl-5-mercapto-4-methyl-3(2H)-pyridazinone as synthesized in the above and 1.4 g (0.01 mol) of methyl iodide were dissolved in 20 ml of dimethylformamide and then added with 2.0 g of sodium carbonate with stirring at room temperature. The reaction liquid was stirred for 3 hours at 70° C. After allowing to cool the reaction liquid was poured into 200 ml of water and extracted with 50 ml of benzene. The benzene layer was washed successively with 50 ml of 10% sodium hydroxide, 50 ml of 1N hydrochloric acid and 100 ml of water, dried over anhydrous sodium sulfate and freed of solvent by distillation to give 2.0 g of a crude product. The crude product was recrystallized from 20 ml of isopropyl ether to give 1.4 g of 2-tert.-butyl-4-methyl-5-methylthio-3(2H)-pyridazinone.

後処理

  1. customThe reaction liquid
  2. stirringwas stirred for 3 hours at 70° C
  3. temperatureto cool
  4. customthe reaction liquid
  5. extractionextracted with 50 ml of benzene
  6. washThe benzene layer was washed successively with 50 ml of 10% sodium hydroxide, 50 ml of 1N hydrochloric acid and 100 ml of water
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationfreed of solvent by distillation
  9. customto give 2.0 g of a crude product
  10. customThe crude product was recrystallized from 20 ml of isopropyl ether

出典と根拠

ORDレコード
ord-7353e3e4b4534911a5dccdc5e40a4a37
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04874861

反応ノート

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