N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-formylbenzenesulfonamide → N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-ethenylbenzenesulfonamide

HRID 1380469ノート

反応式

HRID 1380469 の反応式
C([Li])CCC.[Br-].C1([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)(=[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[CH:13]=[CH2:14])(=[O:42])=[O:43])=[O:39])[N:30]=1

参加物

5

反応物 3

HCID 13097377N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-formylbenzenesulfonamideHCID 21951224Triphenylmethyl phosphonium bromideHCID 178418339Butyllithium

生成物 1

HCID 13772105N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-ethenylbenzenesulfonamide

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 3.7 g of N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]-2-formylbenzenesulfonamide 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 washed with dilute 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 washed with dilute hydrochloric acid, water
  6. customdried
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-4074af18f0884eb8975337af4f039670
出典データセット
uspto-grants-1986_04
特許番号
US04582525

反応ノート

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