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Water → 1-Pyrid-2-yl-2-methylsulphonyl-4-phenyl-pyrazolin-5-one

HRID 1382204
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HRID 1382204 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[C:11](=[O:12])[C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:9][NH:8]1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28].O>O1CCOCC1>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[C:11](=[O:12])[C:10]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[CH:9][N:8]1[S:27]([CH3:26])(=[O:29])=[O:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 135904734-Phenyl-2-(pyridin-2-yl)-1,2-dihydro-3H-pyrazol-3-one

생성물 1

HCID 137867791-Pyrid-2-yl-2-methylsulphonyl-4-phenyl-pyrazolin-5-one수율 71.3%

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

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온도
70 °C

실험 절차

23.7 g (0.1 mole) of 1-pyrid-2-yl-4-phenyl-pyrazolin-5-one are dissolved in 200 ml of dioxane. After addition of 10.1 g (0.1 mole) of triethylamine, 11.5 g (0.1 mole) of methanesulphonyl chloride are added dropwise at room temperature, while cooling gently. The mixture is subsequently stirred at room temperature for a further 2 hours and at 70° C. for 5 hours, cooled and stirred into 1 l of water. The crystals are filtered off with suction, dried in air and recrystallized from ethanol. 22.5 g (71% of theory) of 1-pyrid-2-yl-2-methylsulphonyl-4-phenyl-pyrazolin-5-one of melting point 112°-114° C. are obtained.

후처리

  1. additionare added dropwise at room temperature
  2. temperaturewhile cooling gently
  3. temperaturecooled
  4. filtrationThe crystals are filtered off with suction
  5. customdried in air
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-bdb0565fe646497b876a3bc59c53b61b
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806540

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