Water → HCID 54274887、化合物

HRID 65574ノート

反応式

HRID 65574 の反応式
[CH3:1][C:2]([CH3:28])([CH:7]([NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:20])=[O:19])[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=1)[C:3]([O:5][CH3:6])=[O:4].[H-].[Na+].[CH3:31]I.O>CN(C)C=O>[CH3:1][C:2]([CH3:28])([CH:7]([N:17]([CH3:31])[S:18]([C:21]1[CH:22]=[CH:23][C:24]([CH3:27])=[CH:25][CH:26]=1)(=[O:19])=[O:20])[CH2:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH3:16])=[CH:13][CH:14]=1)[C:3]([O:5][CH3:6])=[O:4]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 53810576HCID 53810576、化合物

生成物 1

HCID 54274887HCID 54274887、化合物収率 96%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A solution of 405 g of methyl 2,2-dimethyl-4-(p-methoxyphenyl)-3-(p-toluenesulphonamido)butyrate in 1800 ml of dry dimethylformamide is added to a mechanically stirred suspension of 52.8 g of sodium hydride in 320 ml of the same solvent. After the reaction mixture has been heated at 80° C. for 1 hour it is cooled when 93 ml of methyl iodide is added. After an additional period of heating (under reflux) the mixture, after being cooled, is poured into plenty of water. A white crystallisate separates. After filtration and drying it melts at 132°-134° C. Yield 96%.

後処理

  1. additionis added
  2. temperatureAfter an additional period of heating
  3. temperature(under reflux) the mixture
  4. temperatureafter being cooled
  5. filtrationAfter filtration
  6. customdrying it melts at 132°-134° C

出典と根拠

ORDレコード
ord-514973f2c1c24851a3cc2d6ede742fab
出典データセット
uspto-grants-1978_12
特許番号
US04128548

反応ノート

読み込み中…