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

HRID 622659
ノート
印刷プレビュー

反応式

HRID 622659 の反応式
[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]
参加物反応条件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 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 135904734-Phenyl-2-(pyridin-2-yl)-1,2-dihydro-3H-pyrazol-3-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-626bc5a71f4b4fdca6f17111997af335
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04772608

反応ノート

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