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Pyridine-2-sulfonyl Chloride → N-[3-(2-acetoxyethoxy)-1-methyl-4-(4-methylphenyl)-1H-pyrazol-5-yl]-pyridine-2-sulfonamide

HRID 1368655
ノート
印刷プレビュー

反応式

HRID 1368655 の反応式
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:12]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)=[C:11]([NH2:20])[N:10]([CH3:21])[N:9]=1)(=[O:3])[CH3:2].[N:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[S:28](Cl)(=[O:30])=[O:29]>N1C=CC=CC=1>[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:12]([C:13]2[CH:14]=[CH:15][C:16]([CH3:19])=[CH:17][CH:18]=2)=[C:11]([NH:20][S:28]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][N:22]=2)(=[O:30])=[O:29])[N:10]([CH3:21])[N:9]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3787675Pyridine-2-sulfonyl ChlorideHCID 222820022-{[5-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-3-yl]oxy}ethyl acetate

生成物 1

HCID 22282030N-[3-(2-acetoxyethoxy)-1-methyl-4-(4-methylphenyl)-1H-pyrazol-5-yl]-pyridine-2-sulfonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To 2-{[5-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-3-yl]oxy}ethyl acetate (Preparation 5) (750 mg) in dry pyridine (5 ml) at room temperature was added pyridine-2-sulphonyl chloride (748 mg), the mixture was stirred for 72 hours. The reaction was concentrated under reduced pressure and the residue re-evaporated from toluene. The residue was then partitioned between ethyl acetate (20 ml) and water (20 ml), dried over magnesium sulfate, filtered and concentrated under reduced pressure to yield the title compound as a yellow solid.

後処理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customthe residue re-evaporated from toluene
  3. customThe residue was then partitioned between ethyl acetate (20 ml) and water (20 ml)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1f2f34c19620477d9d4e992802cf7fba
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06573270B1

反応ノート

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