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

HRID 259052
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HRID 259052 반응식
[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
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참가 물질

5

반응물 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 499178HCID 499178, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-4f5b2dcc8ea64e75918a5d4efbeecabb
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04036631

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