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Water → 4-Benzoyl-4-chloro-2,5-dimethyl-2,4-dihydro-3H-pyrazol-3-one

HRID 259052
ノート
印刷プレビュー

反応式

HRID 259052 の反応式
[CH3:1][N:2]1[C:6](=[O:7])[C:5]([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:4]([CH3:16])[NH:3]1.S(Cl)([Cl:20])(=O)=O.O>C1C=CC=CC=1>[CH3:1][N:2]1[C:6](=[O:7])[C:5]([Cl:20])([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:4]([CH3:16])=[N:3]1
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 24648Sulfuryl chlorideHCID 499178HCID 499178、化合物

生成物 1

HCID 214226054-Benzoyl-4-chloro-2,5-dimethyl-2,4-dihydro-3H-pyrazol-3-one収率 8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of 2.16 g of 1,3-dimethyl-4-benzoyl-5-pyrazolone in 20 ml of dry benzene was added 1.62 g of sulfuryl chloride and the mixture was stirred at room temperature for 4 hours. After completion of the reaction, water was added to the reaction mixture and after shaking an organic layer was separated. The organic layer was washed successively with a saturated aqueous solution of sodium hydrogencarbonate and water, dried over anhydrous sodium sulfate and the solvent was distilled off from the solution. The so obtained residue was recrystallized from n-hexane to give 0.2 g of the desired product melting at 70.5° - 72° C. (Yield 7.6%)

後処理

  1. additionwas added to the reaction mixture
  2. stirringafter shaking an organic layer
  3. customwas separated
  4. washThe organic layer was washed successively with a saturated aqueous solution of sodium hydrogencarbonate and water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off from the solution
  7. customThe so obtained residue
  8. customwas recrystallized from n-hexane

出典と根拠

ORDレコード
ord-4f5b2dcc8ea64e75918a5d4efbeecabb
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04036631

反応ノート

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