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2-Acetyl-N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]benzenesulfonamide → N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-isopropenylbenzenesulfonamide

HRID 235567
ノート
印刷プレビュー

反応式

HRID 235567 の反応式
C([Li])CCC.[Br-].[C:7]1([C:13]([PH3+])([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2C=CC=CC=2)C=CC=CC=1.[CH3:27][O:28][C:29]1[CH:34]=[C:33]([O:35][CH3:36])[N:32]=[C:31]([NH:37][C:38]([NH:40][S:41](C2C=CC=CC=2C(=O)C)(=[O:43])=[O:42])=[O:39])[N:30]=1>O1CCCC1>[CH3:27][O:28][C:29]1[CH:34]=[C:33]([O:35][CH3:36])[N:32]=[C:31]([NH:37][C:38]([NH:40][S:41]([C:25]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[C:13]([CH3:7])=[CH2:14])(=[O:42])=[O:43])=[O:39])[N:30]=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 130972992-Acetyl-N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]benzenesulfonamideHCID 21951224Triphenylmethyl phosphonium bromideHCID 178418339Butyllithium

生成物 1

HCID 13097390N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-isopropenylbenzenesulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

to a stirred mixture of 0.02 mol of n-butyllithium in 20 ml of anhydrous tetrahydrofuran is added 3.6 g of triphenylmethylphosphonium bromide. The above solution is stirred at room temperature for 4 hours. A slurry of 3.8 g of N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]-2-acetylbenzenesulfonamide in 30 ml of dry tetrahydrofuran is then added dropwise. The resulting mixture is refluxed overnight and allowed to cool to room temperature. The precipitate is removed by suction filtration and washed with methylene chloride. The combined filtrates are then washed with diluted hydrochloric acid, water, dried and evaporated to dryness to yield the desired product.

後処理

  1. temperatureThe resulting mixture is refluxed overnight
  2. temperatureto cool to room temperature
  3. customThe precipitate is removed by suction filtration
  4. washwashed with methylene chloride
  5. washThe combined filtrates are then washed with diluted hydrochloric acid, water
  6. customdried
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-ad3d4a6bd3f84cc7818711136a31b6fa
出典データセット
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04640704

反応ノート

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